Documente Academic
Documente Profesional
Documente Cultură
MRC.VER.01-3.12
CONTENT POINTS FOR ATTENTION TO FLAME OPERATION ................................ 3 Safety 1 ................................................................................................................. 5 Safety 2 ................................................................................................................. 7 Chapter 1 Introduction .................................................................................. 14
1.2 Main Features ...............................................................................................................14 1.3 Structure .......................................................................................................................15 1.4 Fundament ....................................................................................................................16 1.5 Performance Characteristics.......................................................................................18 1.6 Models, Specifications and Standard Configuration.................................................19 1.7 Electronic Safety classification....................................................................................21
Chapter 3 Installation..................................................................................... 27
3.1 Acceptable goods ..........................................................................................................27 3.2 Unpacking .....................................................................................................................27 3.3 Installation ....................................................................................................................27 3.4 Acceptance Inspection..................................................................................................38
Chapter 4
4.1 Enter the Software........................................................................................................43 4.2 Edit Analytical Method................................................................................................43 4.3 Setting of Analytical Conditions .................................................................................46 4.4 Selection of Graphite Furnace Conditions (Only for AAS-110A/120A/130A)........51 4.5 Selection of Hydride Generator Method Condition ..................................................52
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4.6 Flame Atomic Emission Method (only for AAS-110A/110B/120A/120B) ...............53 4.7 Modify Existed Method................................................................................................53 4.8 Delete Existed Method .................................................................................................54 4.9 Selection of Analytical Method....................................................................................55 4.10 Analytical Project Design ..........................................................................................55 4.11 Operations...................................................................................................................61 4.12 Flow Diagram .............................................................................................................70
Chapter 5
5.1 Introduction of enriched oxygen air-acetylene flame................................................71 5.2 Operation of enriched oxygen air-acetylene flame....................................................72
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Important:
c. After hearing the solenoid valve sounds, slowly turn the C2H2 flow knob
counterclockwise to 1-1.5L/min. The ignition button should be pressed several times if there is air remaining in the piping. 5. Flame shutdown procedure: Firstly close the main valve of the C2H2 cylinder (clockwise to minimum). After all the C2H2 in the piping is fully burned out, switch off the C2H2 flow. 6. A special C2H2 regulator should be used for C2H2 supply. The C2H2 piping shouldnt be made of or contain Cu, Ag, Hg or their alloys. 7. Before O2 flame operation, operators should study the descriptions in the operation manual carefully. 8. To make an O2 flame, ignite the ordinary flame first. Then slowly increase the C2H2 and O2 flow alternately until the required flame temperature is reached. During the flow increasing, the C2H2 flow should be increased first. Make sure the set oxygen flow will not exceed 70% of the set C2H2 flow and less than 5L/min. 9. To shutdown the O2 flame, decrease the O2 and C2H2 flow alternately. The O2 flow should be decreased first. Make sure the O2 flow will not exceed 70% of C2H2 flow. When it becomes an ordinary flame, The O2 and C2H2 flow knobs should be turned to
follow the procedure in Item 5 to shutdown the flame. its minimum position.
10. Check if the alarm system works well: After igniting the flame, switch off the air supply, the flame should extinguish and alarm should sound; After re-igniting the flame and put a piece of paper in front of the light-control hole on the left wall of the sample compartment, the flame should extinguish and alarm should sound. If there is anything abnormal, shown down the flame and check.
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11. If ignitions according to the instructed procedure cannot be made, contact your local distributor. uses the naked fire for ignition to avoid danger occurs. After switching off the instrument, dont cover the combustion chamber to keep good ventilation.
Dont
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Safety 1
Read this section carefully before using our instrument to avoid person injure or instrument damage accidents occurring. If those accidents occur because of transgressing the operation procedures stipulated in this manual, user should bear responsibility for them. 1.1. If person hasnt been specially trained, the instrument must not be operated. 1.2. Do not install or use this instrument when falling short of the conditions and requirements mentioned in this manual. 1.3. Do not use this instrument in non-AA analysis or test. 1.4. Do not be allowed to install or repair or replace the accessories or software of the instrument without the authority of MRC Corporation. 1.5. To avoid the computer virus attacking the computer and making the system broken down, do not travel on Internet or play games in the computer special used for the analysis. 1.6. Requirements of gas source storage. 1.6.1 It is strictly prohibited that the oxygen steel cylinder and the acetylene steel cylinder can never be put in the same room! The acetylene steel cylinder should be stored in a well-ventilated room without any fire source or hidden fire danger nearby! 1.6.2 Steel cylinders should be stored nearby the laboratory. The distance must be more than 10 meters. The gas pipes should be prevented from impact, squeeze, roast and chemical corrosion. 1.6.3 All steel cylinders should be placed firm and avoid falling down. The gas steel cylinders should be placed vertically. Fire caution must be marked in the room stored the steel cylinders. Fire extinguisher must be equipped in the room. 1.7. Requirements of gases 1.7.1 Acetylene is combustible and detonatable gas, it is very important for keeping good ventilation condition in the room placed the instrument. An evacuating device must be installed above the instrument. 1.7.2 Check all valves and pipes if there is gas leakage before using the instrument. If so, stop using and replace new pipe or new valve. 1.7.3 Before igniting the instrument, check the water seal of the liquid discharging piping is in normal case, otherwise, the fire back will be occurred.
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1.7.4 Be sure that the acetylene switch on the instrument is in the state of OFF before opening the main valve of acetylene cylinder. Open or close the main valve of the cylinders with a special spanner. Do not knock it. The main valve can be turned 1~1.5 circles in maximum. Check the main valve with soap water regularly (three times a week). If the leakage exists, replace it in time. Operation procedures of the oxygen cylinder are the same as the acetylene. 1.7.5 After the analysis, firstly close the main valve on the acetylene cylinder. When the acetylene in pipe is burned out, the instrument can be powered off. Then shut off the acetylene switch and air compressor. Avoid the acetylene left in the instrument. 1.7.6 There is solvent, such as acetone in the acetylene cylinder. If the exit pressure is less than 0.5MPa, it is required to replace a new cylinder to avoid the solvent flow out. The acetylene pressure meter on the cylinder should be checked regularly. Ensure the meter to show the correct output pressure value. 1.7.7 If the humidity in the instrument room is more than 70%, the dehumidify apparatus should be used to make the humidity being less than 50%. 1.7.8 Check if the water seal is good enough before ignition! Otherwise flashback will be occurred. 1.7.9 The cathode metals of some hollow cathode lamps are harmful to human body or pollutant. When they are damaged or obsolete, handle with them according to laboratory standard methods, and do not throw them away randomly.
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The reaction generating acetylene Ag or Acetylene Cu is very sensitivity, so the acetylene and the end-base
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alkyne can be identified by these. The dry acetylene Ag or Acetylene Cu blow up easily when they are heated or be shake and then create metal and carbon.
Ag-CC-Ag
2Ag + 2C + 364KJ/mol
After finishing the experiment, please add the hydrochloric acid immediately to decompose the acetylene to avoid the dangerous. 2.1.3 Chemical stability and reaction activity Chemical stability: instability Harm decomposed material: Hydrogen and carbon. Conditions should be avoided: avoid explosion and whenever cylinders lay down. Using pressure cant exceed 0.1Mpa, the steel cylinder should avoid the temperature higher than 40, and avoid crash and far away from the fire source. Materials should be avoided: oxide, halogen, and halide. 2.1.4 Toxicity: no toxicity but the asphyxia will be caused. Part effect: sensitization. Slow toxicity or long-term toxicity: NPT, IARC, or OSHA Subpart Z hasnt been listed within the carcinogen or incubation carcinogen materials.
(1). The empty cylinder with standard dimension is equipped with air-compressor devices including: safety reducer device, valve and protecting cap. (2). Each cylinder is fulfilled with multi-hole filter material, including: diatomaceous earth, char, asbestos and cement. Acetylene cylinder is filled with packing material and dissolvent (3). Acetone is fulfilled in the cylinder and all of the packing material. The acetone is solvent, it can dissolve the acetylene gas filled in the cylinder. Acetylene gas can be stored and used in the cylinder. (4). According to the requirements, the working pressure should be 1.72Mpa while the temperature is 21 , Originally, when the pressure is reached up to two or three times of the working pressure, make the
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fluid statics detect on the cylinder. The acetylene cylinder should be check and recognized timely. Cylinder body must be re-recognized within ten years from its production. And per ten years it should be recognized. The cylinder body and packing materials only can be recognized by the authorized organizations. (5). The physical description of the cylinder.
Size 1 2 3 4 5
2.3 2.3.1
Cylinder Net weight Gross Weight Gas volume kg kg 21.32 23.81 2.123 31.75 35.83 3.679 45.36 51.26 5.377 79.38 89.70 9.339 83.92 95.14 10.188
m 3
(1). Place the cylinder in the site where is satisfied with the ventilation, safety, and protection against the shine and rain. Temperature of the storage area cant exceed 40, and there mustnt put combustible materials, Strictly prohibit the smoke and fireworks. Keep the distance from stuffed area and urgent exits. (2). The cylinder should be put firmly and upright with proper locked valve outlet cap and valve protection cap. Residual and full cylinder should be separately placed. Using the First in and the first out principle to avoid the overdue of the stored acetylene. Record the inventory regularly. (3) Rotate the valve tightly when it is unused. Far away from heating source, fire source or incompatible materials such as oxide more than 8 meters. Or set a 1.5m high fire wall, which fire prevention speed should not be less than half an hour. (4) Grounded ventilation and electric devices without spark should be used to avoid fire. (5) Regularly check the cylinders for breakage and leakage. Protect the cylinder bottom to avoid contacting damp floor. (6) Make the caution marks on proper places. Treatment and storage should abide principles of inflammable and compress gas.
2.3.2 Transportation:
(1) Forwarders should been trained for carrying such special dangerous materials. (2) Special transportation ways and points for attention: Fixed and standing upright on the truck with well ventilation conditions. Cylinders mustnt be transported in the back case of cars. Make sure that the
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valve cap and the cylinder cap have been re-installed and locked well.
2.3.3 Usage:
(1) For the cylinders, the actions of pull, push, roll or kick all are prohibited. The cylinders should be transported by a specialized barrow. Strictly prohibit hanging the cylinders with cap. Make sure the cylinders are fixed firmly while it is in using. (2) Prohibit to operate the cylinders rudely and unconcernedly to avoid the cylinders and the packing materials to be damaged. (3) Using check-valve to avoid reverse flowing to enter into the cylinder. The cylinder body is prohibited to be heated and far away from the fire. (4) Dont use it unless there is no any Leakages on pipelines and equipments. Before using the acetylene device, check pressure regulator, pipelines and connectors of cylinders with soap water. (5) Steel and wrought iron are recommended for using on the acetylene piping. Pressed-steel, cast-steel, or cast iron device can be used, but pig-iron can be never used any more. Explosive acetylene series may be generated if those materials are used. Pure copper, pure silver or mercury can not be contacted directly with the acetylene. Copper, 70-30 brass or aluminum bronze with damp acetylene will generate the explosive acetylene substance. The weight (not pressure) is used to determine the acetylene quantity. Gross weight (includes cylinder, packing materials, acetone, valve, saturated gas and safety plug, but except for the cylinder cap) is used to subtract the real weight, and then use the difference to multiple 9.1710 to determine the gas quantity in m3 unit. (6) Please slowly turn on the cylinder valve when it has been connected with the instrument. If there is any difficult to open the cylinder, please stop it immediately and inform of the vendor as soon as possible. Dont use tools (such as: screw driver, spanner, etc) to insert the open holes located at both sides of the cylinder cap to open it, otherwise, the cylinder valve will be damaged to cause the gas leakage. Adjustable ringed chain spanner should be used to open the tighten cylinder cap. The cylinder valve cant be turned more than 1.5 circles. In order to decrease quantity of the injection solvent to the minimum, in discontinuous using period, extraction speed of the acetylene should be less than 1/10 of the cylinder volume in per hour; In continuous using, extraction speed of the acetylene should be less than 1/15 of the cylinder volume in per hour. (7) Make sure that the full-filled cylinders are used. The marks must be made clearly on the empty and the residual cylinders so as to identify their using status. - 10 -4
(8) When the cylinder is unused or empty, turn off the valve to avoid the air entry. Please does never use the acetylene gas thoroughly off. Lock the outlet cap of the valve by a spanner after completed the determination. Turn off the cylinder valve, and release the pressures inside of the pressure regulator and the instrument. It is needed to equip the emergency devices to put out fire or deal with the gas leakage. (9) If the surface of the cylinder has sharp or deep depressed, cut, etc, please make marks on the cylinders and inform of the vendor. Any of people can never be allowed to repair the cylinders except for the qualified person from its manufacture. (10) When using the cylinders, safety glasses, safety shoes and normal gloves should be put on the operators.
(4) Regularly check the pipelines, connectors and valves for the gas leakage. Repair it properly if there is the gas leakage existing. (5) If the concentration of the copper, silver and mercury are very high, dilute it as possible as it can be within the allowance range of the instrumental sensitivity. (6) When determining the high concentration samples such as: copper, silver or mercury, sucking and spraying solution time should not be so long. Spray promptly the de-ion water for 5~10 minutes after completing to suck in the sample per time. (7) After completing all the determinations, absorb and spray the de-ion water for 20 minutes more or less with the flame. (8) Regularly (once a week) clean the nebulizing system to eliminate the residual samples with the high concentration. (9) During the analysis, if hearing some slightly explosion sound or any other abnormal sound, promptly the flame is off, and then check every part of the nebulizing system. (10) When the flame operation is selected, users should try the best effort to avoid compression, crashing or other pressure impact.
SCBA. (5) Product yield after combustion: CO and CO2. 2.3.5.2 Emergent treatment of abnormal leakage. (1) All of people and cars must escape far away from this area. (2) Use suitable fire-proof equipment. (3) Check the concentration if it is higher than 2.5%, if it is so, the fire and the explosion will be occurred immediately. If the concentration is higher than 10% of the low explosion limit, people and carriage are prohibited to enter this area. (4) Eliminate all of the fire sources; use the maximum size of explosion-proof ventilation device. And cut off the leakage source if it is possible. (5) Separate the leaked container. (6) Inform of the vendor if the cylinder is leaked. (7) If the pipeline inside of the instrument occurs the gas leakage, close the cylinder and discharge the pressure safely. Blow the pipeline with inert gas before repairing.
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Chapter 1 Introduction
1.1 Applications
Atomic Absorption Spectrophotometer (AAS) is a kind of instrument for the inorganic analysis. It is widely used in environmental protection, medicine, sanitation, metallurgy, geology and petrochemical industry fields for micro and trace analysis. Atomic Absorption Spectrophotometer can analyze more than seventy kinds of elements. With the development of instrument accessories and analyzing technology, more objects, from element to morphology and from nonmetallic anion to gas-phase molecule, could be analyzed directly or indirectly.
1.2.2 Enrich oxygen flame analysis technique. Models AAS-110A/110B instruments adopt an enriched-oxygen air-acetylene flame atomization system (patent No: 92101560.7) for the first time in the world. The flame temperature changes continuously from 2300 to 2950, so it can substitute for N2O- acetylene flame when analyzing the elements with the high temperature and it is more safety and conveniently-used. Enrich-oxygen air-acetylene flame is much better than the air-acetylene flame and the N2O-acetylene flame when analyzing the elements with the high temperature such as: Ca, Sr, Ba, Eu, Yb, Mo, Ga, Sn, etc. 1.2.3 Data processing Data processing will be performed in computer. Absorbance standard deviation, relative standard deviation, working curve and instantaneous signal graph will all be shown on the monitor. The working curve and instantaneous signal graph can be printed out. The multi-instantaneous signal overlapped graphs can be displayed in order to view the variation of the instantaneous signal. 1.2.4 High sensitivity The characteristic concentration of the flame method is in the range of mg/L to g/L (characteristic concentration of Cu is less than 0.04mg/L/1%). The characteristic quantity of the graphite furnace method is in the range of 10-9 to 10-12 g(The characteristic quantity of Cd is less than 110-12g). 1.2.5 HCL power supply system with high performance. Models AAS-110A/110B/120A/120B can use the hollow cathode lamps with the high performance, which have higher intensity and lower background. The intensity of the hollow cathode lamp with the high performance is about 3 to 15 times higher than that of the common hollow cathode lamp, so it is helpful to improve the performance of the instrument. 1.2.6 Photo-electronic temperature-controlled system (for models AAS-110A/120A/130A). FUZZY-PID technology is adopted with the double-curve mode. Its advantages are: fast heating up speed, accurate stable temperature-controlled and temperature auto-correction function. It also has high adaptability for the environment and its temperature-controlled accuracy cant be affected by the live wire wave and the resistor change of the graphite furnace.
1.3 Structure
1.3.1 Main unit: It consists of light source chamber, sample compartment, monochromator, gas pipeline box and electronic box.
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1.3.1.1Light source chamber: The hollow cathode lamps and the deuterium lamp are mounted inside of the light source chamber. For AAS-110A/110B/120A/120B, six HCL lamps mounted can be ignited at the same time and automatically change-over randomly. For AAS-130A/130B, four HCL lamps mounted can be switched on at the same time and auto-changeover randomly. 1.3.1.2 Sample compartment: It is used to install the atomizer. Models AAS-110A/120A/130A are provided with the flame and the graphite furnace atomizer together as a whole body of the instrument. When changing the analytical method, use the keyboard of the computer automatically to change over between the flame and the graphite furnace. Rotate the switch valve to change the locking state of the graphite
tube. Models AAS-110B/120B/130B all are the flame atomizer. 1.3.1.3 Monochromator: CT type grating monochromator is adopted in the instrument. It consists of optical system, sine mechanism of wavelength scan system; and automatic adjustable slit system. 1.3.1.4 Control system of gas pipeline: For AAS-110A/110B, it consists of three gas piping: air, acetylene and oxygen gases. For AAS-120A/120B/130A/130B, there are only two gas piping, such as: air and acetylene gases. 1.3.1.5 Electric Box: Provides with an electric control system. 1.3.2 Computer: It is used as a data processing system and equipped with the printer, which can print out the analysis data. 1.3.3 Power Source of Graphite Furnace: It is used to supply the atomizer of the graphite furnace. The techniques of the photo-control temperature and FUZZY-PLD are adopted to make the atomizer of the graphite furnace quick and stable rising temperature.
1.4 Fundament
1.4.1 The fundament of the instrument is that the characteristic spectrum of the element to be measured is emitted from the light source and absorbed by the ground state atoms of the same element in the sample steam when passing through the flame or the non-flame atomizer. Determine the energy variation of characteristic wavelength radiation light, and then the content of the element in the sample is obtained. 1.4.2 The fundament of S-H background correction technology is described as the followings. The light source (hollow cathode lamps) is powered by two kinds of cyclical pulse current with different width and amplitude. During the wide pulse and low current, the emitting spectrum of the hollow cathode lamp has a normal spectral line width. While during the narrow pulse and high current powering, the emitting spectrum band is wider and various self-absorptions occur. Background absorption is caused by molecule absorption and light scattering, which belongs to wide band absorption. It is not affected by widening emitting spectrum and self-absorption, so it keeps the same absorption for both normal spectrum and self-absorption spectrum. However the absorption of the to-be-measured element atoms in the sample is seriously decreased when the emitting spectrum is widened and self-absorption occurs. So the normal spectrum signal includes atomic absorption + background absorption, while the self-absorption spectrum signal includes little atomic absorption + background absorption. The difference value between them is the atomic absorption signal with background correction. For details about this technology, refer to the reference books. 1.4.3 Operating procedures of the instrument (1) The main unit is connected with the computer, ignite the hollow cathode lamp(HCL) selected by the computer; (2) The HCL radiation light modulated by the pulse is passed through the monochromator of the atomizer; (3) The monochromator will select the radiation light of the characteristic spectrum of the element to be determined is entered into the photomultiplier (PMT) to transfer the optical signal to the electric signal and send it to the computer; (4) The computer automatically adjust the negative high voltage value of PMT (gain), thus the light energy adjustment of HCL (AA) is 100%; (5) Use the flame method or the graphite furnace method to make the element to be determined in the sample forming into the ground state free atomic vaporization, absorb the radiation light of the characteristic wavelength of the element to be determined emitted from the HCL; (6) The variance of the light signal after passing through the photo-electric detecting system is transferred to the variance of the electric signal to the computer; (7) The computer will calculate the absorbance value of the sample - 17 -
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1.5.6 Linearity of Standard Curve Flame method; Linear range of the standard curve is less than 0.6Abs; Linear Correlation coefficient : r0.995
air-acetylene flame, enriched-oxygen air-acetylene flame, flame emission, D2 lamp background correction, S-H background correction. Six lamps of auto-changeover, auto-peak picking, auto-wavelength air-acetylene scan, incorporated emission, atomizer, D2 lamp
flame,
flame
atomizer.
enriched-oxygen air-acetylene flame, flame emission, D2 lamp background correction, S-H background correction.
Six lamps of auto-changeover, auto-peak picking, auto-wavelength scan, air-acetylene flame, flame emission, D2 lamp background correction, S-H - 19 -
atomizer.
background correction. Main unit, Computer, printer, AAS-130B Air compressor, flame Four lamps of auto-changeover, wavelength setting, auto-wavelength scan, air-acetylene flame, D2 lamp background correction.
1.6.1.2 Light Source: Hollow Cathode Lamp, D2 Lamp Modulation Mode: Square Wave Pulse Modulation Frequency: 400Hz (No background correction mode or No D2 lamp background correction mode) 100Hz (S-H background correction mode) 1.6.1.3 Optical system: Czerny-Turner Monochromator Grating: Plane diffraction grating with 1800lines/mm Blazed wavelength: 250nm Focus: 277mm Band-width: 0.1, 0.2, 0.4 and 1.2nm Wavelength Adjustment mode: Wavelength setting, Wavelength Scan, auto-peak picking (Except for AAS-130A/130B). 1.6.1.4 Photometric mode: Single beam 1.6.1.5 Atomization System: Flame atomizer (Only for AAS-110B/120B/130B) Pre-mixed 100mm single slot burner Incorporated Atomizer (Only for AAS-110A/120A/130A) Ignition Mode: Automation Flame emission burner (Only for AAS-110A/110B/120A/120B) Hydride method (Option: Hydride generator) 1.6.1.6 Safety System: Safety protection and alarm for flame off Safety protection and alarm for ignition failure Safety protection and alarm for air pressure relief - 20 -
Safety protection and alarm for gas leakage 1.6.1.7 Data Processing System: Measurement mode: Absorbance, Concentration, Content and Emitting Intensity. Read mode: Instantaneous value, peak high value, integral value, peak area value. Display mode: Data, signal graph and fitting curve. Signal Processing Function: Standard curve method; Standard Addition Method; Standard sample numbers (option from 1 to 10), Re-slope and statistical Average etc. Information Memory Mode: Working Conditions; Analyzing Data Table; Analyzing Reports and Signal Outline. 1.6.1.8 Power Requirements: 220V/110, 50Hz/60Hz, 200VA 1.6.1.9 Instrument Dimensions: 102 (L)49 (W)54 (H)cm 1.6.1.10 Weight: 80kg
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2.3.3. Ground
For the instrument well running and safe operation, the earth wire of this instrument should be connected to a metal board buried 1.5m under the ground.
adjustor. The outlet pressure should be 0.05MPa0.07MPa when using the air-acetylene flame operation, and the outlet pressure should be 0.08MPa0.1MPa when using the enrich-oxygen air-acetylene flame operation. The acetylene purity must be 99.6% more. It is necessary for the flame operation. Argon gas: The cylinder filled with the argon is used with a specialized decompress adjustor The inlet pressure should be 2.5MPa and the outlet pressure should be adjusted in the range of 00.4MPa. The argon purity must be 99.99%. It is necessary for the graphite furnace operation or the hydride method.
4 Oxygen gas: The cylinder filled with the oxygen is used with a specialized decompress adjustor. The
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outlet pressure should be 0.1MPa0.12MPa. It is necessary for the enriched-oxygen air-acetylene flame method. 2.3.2.2 Storage Requirements
1 The acetylene cylinder should be stored in a well-ventilated room without any fire source nearby! It
should be also placed near to the laboratory. It is strictly prohibited that the oxygen and the acetylene cylinders area placed together!
2 The cylinders of safety gas and air compressor may be placed in laboratory. 3 All cylinders should be placed firmly, which is stable without the declination.
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2.4.1.2 Working bench should be firm without changing shape after load-bearing. 2.4.1.3 The surface of the working bench should be flat, and covered by a shockproof corrosion-resisting plastic or rubber board. 2.4.1.4 When putting the work-bench, remain a certain space around it in order to connect the gas pipes or examine and repair the instrument conveniently. 2.4.2 Keep the room cleaning, stable temperature. A conditioner should be installed if it is possible. 2.4.3 The laboratory for putting the atomic absorption spectrophotometer must be separated from the chemistry laboratory so as to prevent the instrument from acid, alkali and other corrosive gases, steam and - 25 -
smog. 2.4.4. For trace analysis or super trace analysis with the graphite furnace method, the requirements of the cleanness in the laboratory are more strictly regulated. Generally, the indoor air pressure is positive and the air should be filtered. The floors and walls are decorated with dustproof materials. Especially when analyzing those easy-polluted elements, such as calcium, kalium, sodium, magnesium, zinc, etc, the laboratory can only be decorated with the inert plastic and Teflon materials. To obtain accurate results, be careful when touching vessels with sample solutions and be sure that the sample solution has not been polluted yet. 2.4.5 .In order to avoid the virus, the computer connected with AAS is not allowed to be connected with the internet or the other program
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Chapter 3 Installation
3.1 Acceptable goods
Check the goods when receiving them. Make sure that the name and quantity of the goods are in accord with the contract signed. Check if the packing boxes are damaged. If it is so, please negotiate it with the forwarder and inform of the manufacturer immediately.
3.2 Unpacking
3.2.1. Unpack the boxes and take out all of the documents packed in it. Check if the accessories of the instrument are all correct and complete according to the packing list. Meanwhile check if there is any damage on the instrument after a long transportation. If it is so, please contact the concerned department and inform of the manufacturer immediately. 3.2.2. Read all the operation manuals of the instrument carefully and learn the fundament, structure and operation of the instrument. 3.2.3. Prepare the working conditions and necessary laboratory devices according to this manual, and install the instrument according to this chapter. 3.2.4. Test the main performance of the instrument. The acceptance of the instrument should be made with the concerned specialized engineer together.
3.3 Installation
Before the installation, prepare all necessary conditions and devices in the room which will be installed the instrument. Put the instrument on the working bench, and then install and adjust it according to the instructions mentioned in this manual.
user should prepare some screwdrivers with various sizes, shifting spanners, sharp nose pliers, and so on.
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Fig. 3-1 the connections of outer electric systems with the main unit
Adjust method:
Ignite HCL and adjust its position well; Put a hard white paper above the burner (shown as in Fig. 3.2) to observe the gathering light spot of the hollow cathode lamp, and then move the burner to make the light spot exactly located on the burner slot. Parallel move the paper, and rotate the angle of the burner to make the light spot aimed at any position of the burner slot.
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the following:
1 C2H2 OUTLET C2H2 INLET;
Oxygen INLET
The connections are shown in Fig.3-3 (dot line part in the diagram shows that the pipes have been connected well before the delivery). (2) The gas control unit of the main unit is connected with the atomizer by 6(outer diameter)1mm colorful nylon tube. And white, blue and yellow color tubes are respectively used for the acetylene, the oxygen and the air in the gas control unit. 3.3.4.2 Connections of Gas Pipes only for Model AAS-120B/130B: There is a gas control unit and four joints at the rear of the instruments. Four jointers are respectively: Inlets and outletsof acetylene (C2H2) and air. The connection method also refers to the Fig.3.3. The difference with Model AAS-110 is no oxygen piping. (1) Gas pipes of the flame atomization system, including acetylene, oxygen and air, are connected as the following: 1) C2H2 sources OUTLET C2H2 INLET; C2H2 OUTLET C2H2 INLET of atomizer. 2) Air compressors OUT AIR INLET ; AIR OUTLET AIR INLET of atomizer; (2) The gas control unit of the main unit is connected with the atomizer by 6(outer diameter)1mm colorful nylon tube. And white, blue and yellow color tubes are respectively used for the acetylene, the oxygen and the air in the gas control unit.
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operation
of
integration
atomizer
only
for
models
3.3.5.1Structure of the integration atomizer and operation of the keyboard Atomizer used on AAS-110A/120A/130A adopts an integration designing. The atomizers of the flame and the graphite furnace have been mounted well on the main unit before the delivery. Both positions can be changed over by a small keyboard located at the front end of atomizer. There is no need for the user to do it by itself any more. Operation method of the integration atomizer When selecting the flame analysis or the graphite furnace analysis, the corresponding atomizer should be moved to the center of the optical path. The auto-changeover can be realized by the small keyboard at the front end of the atomizer as shown in Fig. 3-4.
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UP
FRONT
BACK
DOWN
FLAME
FLAMELESS
graphite furnace vertically (by pressing UP and DOWN keys) to search the maximum position of the lamp energy until the optimal position is found out. Press FLAME key after powering on, the height from the top of slot sheet of burner head to the center of the optical path is 7mm. Press FLAMELESS key, the acquiesce position of the graphite furnace is still the center of the optical path. If the flame atomizer is currently located in the center of the optical path (or graphite furnace atomizer), the moment press FLAME key (or FLAMELESS key), there is no any response from the instrument, it is especially designed for preventing the repeated action, it is in normal case. Before switching on the main unit, the atomizer currently located in the center of the optical path is just one to be used, so it is not necessary to press the concerned keys to select it again. But if the position is required to be fine adjusted, again press FLAME key or FLAMELESS key. 3.3.5.3 Connection of gas pipes for integration atomizer (only for AAS-110A) The rear of the gas controlling box is located at the left back of the main unit of AAS-110A, including six jointers on it, they are respectively inlets and outlets of Acetylene, oxygen and air, marked with characters or ion (the same as AAS-110B). The rear of the integration atomizer is located at right rear of the instrument. All of interfaces are shown in Fig.3-5, with the characters marked. Among them, a hole of the flame pipe has the extension nylon tubes with yellow, white and blue colors. One ends of them have been respectively connected to air inlet of nebulizer, auxiliary combustion gas inlet of atomization chamber and fuse inlet of atomization chamber, the connection method for other ends of them extended to the outer side of the instrument are shown in Fig. 3-5. The gas pipes of the flame atomization system are divided into three parts: acetylene, oxygen and air. The connection methods are the same as AAS-110B. The gas pipe of the main unit is connected with the atomizer by a color nylon tube with 6 X 1mm. AS same as the inter side of the gas controlling case , acetylene, oxygen and air are respectively corresponding to white, blue and yellow nylon tubes. Note: Gas box of the main unit must be connected with the oxygen pipe between the tube and incorporated atomizer. 3.3.5.4 Piping connections of integration atomizer with flame operation for AAS-120A/130A There are four jointers located at the rear panel of the gas control box, they are respectively: Inlets and outlets of acetylene and air as shown in Fig.3-5. - 33 -
Fig. 3-5 Gas Pipes Connections of Flame Atomization System (AAS-110A Type) The gas piping of the flame atomization system consists of two pipes of acetylene and air. Its connections are as same as the AAS-120B/130B AAS. A. Outlet of acetylene source---Fuel gas inlet Fuel gas outlet--- Fuel gas inlet of atomization chamber B: Outlet of air source---Air inlet Air outlet---Air inlet of nebulizer The gas piping of the main unit is connected with the atomizer by a color nylon of 6 (OD) X 1mm. As same as the inside of the gas control box, the white and yellow nylon tubes are respectively used for the acetylene and the air. 3.3.5.5 Piping connections of the graphite furnace atomization system only for AAS-110A/120A/130A The graphite furnace atomization system consists of integrated graphite furnace and power supply of graphite furnace. The graphite furnace system includes the connections of electric circuit, gas piping and water piping. All of the connections above mentioned must be ready before the operation. Details refer to the instructions of the graphite furnace system. 3.3.5.6 Mounting and dismounting the graphite tube: The following operations cant be done unless the gas pipes of the graphite furnace power supply have been well connected and the argon cylinder has been ready opened. During dismounting the graphite tube, please
- 34 -
refer to Fig.2-1 in the operation manual of the graphite furnace system. Rotate the rotation switch valve as shown in Fig 2-1 counterclockwise, cut off the gas of the cylinder, and then pull out a certain distance of the right cavity of the graphite tube, the moment take off the graphite tube. The procedures for mounting the graphite tube is just reversely procedures with dismounting it above mentioned. Firstly mount the graphite tube, push the right cavity to the left side tightly and again clockwise rotate the rotation switch valve shown as Fig2-1, open the pressure of the gas cylinder, make two cavity bodies contacted tightly, that shows its installation is complete.
- 35 -
Fig. 3-6 Installation of Gas-water Separator 3.3.7.2 The gas-water separator equipped with the air-compressor is connected well in series and hang it on the water discharge holder (pay attention to the direction of the arrow). 3.3.7.3 Connect the Air outlet of the tube to the Air inlet of the main unit, and then connect the Air inlet to the Air outlet of the air compressor. 3.3.7.4 After the air compressor running, do drain off when the water in the gas-water separator overruns 1/3 of the whole volume. 3.3.7.5 Drain off procedure: Place a container below the gas-water separator, and then unscrew the water discharge valve to drain off the water. Screw it again when the water is over. 3.3.8 Installation of acetylene source Do read the safety (1) and (2) in the manual. 3.3.8.1 The acetylene cylinder should be placed outside of the Laboratory, with the good ventilation. The qualified piping must be used to lead it into the Laboratory. Place a fire proof warming notice at the acetylene source and provide a fire extinguisher there. NOTE 1: NO OPEN FLAME OR OVER-HEATED OBJESTS AROUND THE
ACETYLENE SOURCES! NOTE2: DO NOT PLACE ACETYLENE SOURCES AND OXIDATIVE GAS SOURCES TOGETHER! 3.3.8.2 Acetylene cylinder must be equipped with special pressure regulator. Use the specialized tools to open or close the main valve of the acetylene cylinder.
- 36 -
The acetylene cylinder should be placed vertically and firmly to avoid falling down.
3.3.9.2 NEVER PLACE THE OXYGEN CYLINDERS AND THE ACETYLENE CYLINDERS
TOGETHER! Note: Model AAS-110A/110B needs the oxygen source, and Model AAS-120A/130A is not required any more.
- 37 -
condition when analyzing with the flame operation!!! 3.3.11. Inspection of Gas Leakage When the installation of flame atomization system is completed, before running the instrument, do check if any pipeline junctions or parts of the gas control unit have gas leakage. Especially check if the explosion-proof film at the rear part of the atomization chamber of the burner is well sealed, otherwise, the flashback is easily occurred when igniting the flame. It is very danger! NOTE: KEEP THE SPARE EXPLOSION-PROOF FILMS WELL FOR THE FUTURE USE.
3.4.1. Items of Acceptance Inspect the main specifications mentioned in Chapter One. 3.4.2. Requirements of Acceptance 3.4.2.1 The instrumental acceptance should be made in accord with the requirements of the working environment mentioned in Chapter. Otherwise due to the extreme conditions, the troubles may be caused or the results can not meet the requirements stipulated in this manual. 3.4.2.2 The acceptance should be according to the following operation guide. 3.4.3 Method of Acceptance 3.4.3.1 Wavelength Range and Wavelength Accuracy
1 Wavelength Range
Use Cu lamp to inspect the wavelength of 205.5nm at the short wave; Conditions: Wide pulse lamp current: 3mA; Spectral band-width: 0.4nm; Requirements: When the spectral intensity makes the energy up to 100, the high voltage of PMT (gain) is less than 600V; Use Hg hollow cathode lamp to inspect the wavelength of 871.6nm at the long wave; Conditions: Wide pulse lamp current: 3mA; Spectral band-width: 0.4nm; Requirements: When the spectral line intensity makes the energy up to 100, the high voltage of PMT (gain) is less than 600V. Wavelength Accuracy Use Hg hollow cathode lamp to inspect the wavelengths of 253.7nm, 546.1nm and 871.6nm Method: Select Hg element and position number of the lamp; Spectral band-width: 0.2nm; and then input the above three wavelengths respectively and click the Auto- wavelength button. The software will automatically seek the peak position and show the wavelength value. (NOTE: For model AAS-130/130A, click wavelength setting to find out the maximum energy value by fine adjustment). 3.4.3.2 Resolution Use Mn hollow cathode lamp to check the wavelengths of 279.5nm and 279.8nm; Conditions: Wide pulse lamp current: 3mA; Spectral band- width: 0.2nm Requirements: The energy ration between the wave hollow and the wave peak is less than 40% that shows it is qualified. Method: Select Mn element; Select the wavelength of 279.5nm in Instrument condition page. Click - 39 -
Auto-wavelength (click wavelength setting for AAS-130A/130B). When the seeking peak is over, select the wavelength in the range of 279.0~ 280.5nm on the wavelength scan page. When it is over, seek the first peak (maximum peak) and the nearby wave hollow, record each energy. The wave hollow value should be reached up to the specifications stipulated in the manual. 3.4.3.3 Stability Measure the static base-line stability: Conditions: Use Cu hollow cathode lamp to check the wavelength of 324.8nm with any of the lamp number; Spectral band-width: 0.2nm; Wide pulse lamp current: 3mA; Damp constant: 2. Warm up the instrument for half an hour, and then find out the maximum energy. Refer to the section 4.10.6, click the stability icon on the left of measurement page in tools column to appear the window of the baseline stability as shown in Fig. 4-19. Select the time length of 30minutes and after zeroing, start the measurement. The sampling precision can reach up to 0.001Abs. When the energy is 100 more or less, directly compare the drift to that mentioned in the section 1.5.4. 3.4.3.4 Characteristic Concentration (or Characteristic Quantity), Detection Limit and Precision determination. Only one element is required for inspecting the determinations of Characteristic Concentration (or Characteristic Quantity), Detection Limit and Precision determination. Determination of Characteristic Concentration (or Characteristic Quantity), Detection Limit and Precision of Cu element with the flame method: Conditions: Cu, 324.8nmSpectral band-width: 0.4nm; Damp constant: 2; Other parameters are adjusted to the best optimal state. Determining method of Characteristic concentration and detection limit: Cu standard solution: 1.0g/mL; Blank solution: 0.5% HNO3 water solution Select the blank solution on the Working curve parameter page; Measure the blank times: 20; Input 1.0 in standard sample table; Measuring times of the sample: 3; Select the unit of the concentration: g/mL or mg/L. Firstly the blank measurement is made and the standard samples are made afterwards. After the measurement, the characteristic concentration and detection limit will be calculated automatically. Determination of precision: Cu standard solution: 3.0g/mL; Blank solution: 0.5% HNO3 water solution In the standard sample table, input 3.0 and repeat times: 11; and do not select the blank measurement. The - 40 -
unit of concentration is g/mL or mg/L. After the measurement, the precision for 11 times measured will be calculated automatically. Linearity of Calibration Curve Conditions: Cu: 324.8nm; Spectral band-width: 0.4nm; Damp constant: 2; Other parameters are adjusted to the best optimal state. Cu standard solution: 1.0, 3.0, 5.0g/mL; Medium is 0.5% HNO3 water solution; Blank solution: 0.5% HNO3 water solution In the standard sample table, input 1.0, 3.0, 5.0g/mL, and respectively measure the blank solution and those standard solutions, and then set up the standard curve. The linear correlation coefficient should be more than 0.995. Ba characteristic concentration and detection limit with the enrich-oxygen air- acetylene flame method: NOTE: THIS ITEM IS ONLY FOR AAS-110A/110B. Conditions: Ba: 553.6nm; Spectral band-width: 0.4nm; Damp constant: 2; The other parameters are adjusted to the best optimal state. Ba standard solution: 5.0g/mL; Blank solution: 0.4% KCl water solution In the standard sample table, input 5.0 and repeated times of the sample: 3; The unit of concentration is g/mL. After the measurement, the characteristic concentration and the detection limit will be calculated automatically. Determination of Characteristic quantity and precision with the graphite furnace method: Conditions: Cd: 228.8nm; Spectral band-width: 0.4nm; Cu standard solution: 1.0g/mL; Sampling volume: 20L. Atomization conditions: Dry temperature: 80~100 C; Dry time: 20sec; Slope: 10sec; Ash temperature: 240 C; Ash time: 15sec; Atomization temperature: 1800~1900 C; Atomization time: 3sec.(Conditions mentioned above are only for reference). Sampling: In the standard sample table, input 1.0g/L and repeat times 7, and select the blank measurement. Suck in 20L standard solution with concentration of 1.0g/L with a min-syringe and inject it into the graphite furnace. After the measurement, the characteristic quantity and Precision value will be calculated automatically. 3.4.3.5 Inspection of Lamp Turret - 41 O O O
Model AAS-110A/120A instruments can be provided with six lamps and Model AAS-130A/130B is provided with four lamps. Every lamp should be powered on and inspected. The operation procedures
refer to the concerned section in this manual. Note: (1) Standard solutions should be prepared just before the measurement. Long time storage will cause the concentration error. (2) Various pollutions must be avoided during preparing the standard solutions, otherwise, the results will be abnormal. (3) The measurements of the characteristic concentration and the detection limit are effected greatly by the analyzing conditions and instrument parameters selected. Whether for the flame method or the graphite furnace method, when the abnormal results occur, re-adjust flame performance, flame height, spray status, atomization conditions and function parameters in order to get better results. 3.4.4. Proposal of the acceptance results Inspection records should be made when the acceptance inspection is executed. If any function is in abnormal case, please inform of the local dealers.
- 42 -
Fig.4-1
element and then click OK. This element has been selected and return to the page of Fig.4-3. The Method description can be input by the user or without anything. When everything is OK, click OK to appear the page as shown in Fig.4-5.
- 44 -
Fig. 4-2
Fig. 4-3
Fig. 4-4 - 45 -
This wavelength is the main sensitive line of the element to be analyzed. If you want to analyze the second sensitive line, please input the wavelength manually.
2 Hollow cathode lamp: There are two kinds of the hollow cathode lamp providing: Common hollow
cathode lamp (HCL) or high performance hollow cathode lamp (HPHCL). Note: The HPHCL can be only used on the position number of 5th or 6th lamp# for Models AAS-110A/110B/120A/120B, which provide with the six lamps, while AAS-130A/130B are not available. Position of hollow cathode lamp: There are six lamp positions available for the selection after clicking the drop list of the menu. But pay attention to that the hollow cathode lamp selected here must be in a accord with the element selected in the element period table. Otherwise the accuracy of wavelength and energy will be decreased.
4 Background corrector: D2 lamp method or S-H method is available. 5 Slit, Main (lamp current): Input the spectral band-width and the lamp current according to the
different elements.
6 Warm-up current: Input different current to warm up the lamps and prepare for the next analysis. 7 Aux. current: It is used to supply the HPHCL. Only if the HPHCL is selected, this current could be
input to increase the sensitivity of the analytical element. D2 current and SH pulse current : D2 lamp current and SH pulse current can not be inputted unless D2 lamp current and SH pulse current have been selected in the Background corrector.
- 46 -
Fig. 4-5
method.
3 Read delay: Only for Graphite furnace method. It is the time interval of the time from starting to
appearing peak.
4 Read time: Only for the flame method or the hydride method. It shows the sampling speed. 5 Damp constant: It is used to decrease the noise and generally select it to be 2. 6 Smoothing: Only for graphite furnace method. It is used to make the curve smooth. shows that it is
selected.
- 47 -
Fig. 4-6
Fig. 4-7
- 48 -
2 Conc. unit: g/mL or ng/mL. 3 Sampling volume: Only for graphite furnace method. Standard sample and unknown sample volume is
generally 20L.
4 Conc.: Ten standard sample points can be inputted such as: S1, S2, S3S10. 5 Rep: Measurement times of standard blank and standard sample. It shows the measuring times of the
standard blank and the standard sample points. The average value obtained after these measurements will be participated with the curve fitting.
6 STD blank: Click Multiple selective frame located at the side of the standard blank to be , that
shows the standard blank is selected as shown in Fig. 4-7. It shows that the STD blank is deducted when measuring the standard sample points per time. If clicking the multiple selective frame to delete , that shows that the standard blank is not selected. It means that the zero point is forced to be passed through. The moment, S1 is inputted as the standard blank, again sequentially input the sample point. For example: the standard sample points are 1g/mL, 3g/mL and 5g/mL. During inputting, respectively use the mouse to click S1 to be 0, S2 to be 1, S3 to be 3 and S4 to be 5. NOTE: On this page, if the other concentration does not input the concentration value, must be made at the standard blank, otherwise, Method library to be blank is appeared, so the program is automatically ejected
- 49 -
Fig. 4-8
1 Flame type: AirClick the Flame condition tab in Fig.4-5, and appear the page as shown in Fig.4-8.
Acetylene (For Model AAS-110B/120B/130B) or Enriched-oxygen air- acetylene type (For Model AAS-110A) is selectable.
2 Acetylene flow, Air flow, Oxygen flow, Height of burner: These parameters can be inputted
referring to the analyzing manuals and the result report also can be printed out.
multiple selective frame to make showing in the frame. That shows that the re-slope can be automatically inserted in the set sample table.
2 STD interval of re-slop inserted: If selecting and inputting the auto-re-slope and the interval of the
auto-re-slope, the re-slope will be automatically inserted according to the interval being set in the edited sample table.
3 STD concentration of re-slope: The user can select and input by itself, or select and input from the
standard sample table. Select it with clicking select from STD table. After completing all the settings, click OK to return to the page of Fig.4-2. Click Finish to complete the method editor.
- 50 -
Fig. 4-9
Fig. 4-10 Refer to Fig.4-2, click Graphite furnace AAS and Create, next operations will refer to the sections of 4.2 and 4.3, the difference is that Flame method is changed into Graphite furnace Method in Fig. 4-5 as - 51 -
shown in Fig.4-10. Working process of the graphite furnace is divided into three steps: dry, ash and atomization. The temperature, ramp time and hold time are differed according to the various elements. Refer to the operation manual of the graphite furnace. Double click the table to input the value.
1 Main gas: If this column is blank, the main gas is open in this step. If inputting 0 into this column,
main unit during the last three seconds of ash step or the first three seconds of atomization step.
3 Photo-control: Double click this column to show ,it means that the photo-control mode is selected
in this step. Otherwise, constant voltage heating mode is selected in this step.
4 Carry-gas flow: Get in the frame ,that shows it is selected. 5 Matrix improver: Input the matrix improver type in the frame so as to print out the report.
When all the above settings are over, click Check and OK, and then the page will be returned to Fig.4-2. Click Finish, the method edit is completed.
conditions of the element to be analyzed. The analyzing operations are the same as the flame AA method.
- 52 -
Fig. 4-11
- 53 -
Fig. 4-12
Fig. 4-13
Fig. 4-14
- 54 -
Fig. 4-12. If any of the existed method is required to be deleted, double click it to show the blue color, click OK to delete it. The page will go back to Fig.4-2.
Fig. 4-15 Refer to Fig.4-14, click Sample table to appear Sample Information page as shown in Fig.4-15.
1 No.: Number of unknown samples. 2 Name: Name of unknown samples. 3 Quantity ml and Dil.Vol (ml)(dilution volume): If sampling quantity is 1ml, the diluted volume
should be 50ml, the dilution multiple is 50X. If all the sample names, sampling quantity and the diluted
- 55 -
volume are the same, the numbers input can be following: For example, there are 15 unknown samples, click the series number column to input 1, , 15 into No column and input GGS into the Name column, and respectively input 1 and 50 in Quantity column Dil.Vol column, and then click Expand button. All the samples will be automatically numbered in order.
4 Append: Click Append continuously to edit the sample information at the end of the sample table.
If the sample name, quantity and diluted volume are all not the same, click Append to input the corresponding number, sample name, quantity and diluted volume.
5 Clear: It is used to clear all the items in the sample table. 6 Batch No.: The sample batch number. 7 Type: Sample type such as: liquid or solid.
After inputting all the information of sample table, click OK, and return to the page as shown inFig.4-14.
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(gain) of PMT until the energy is in the state of 100% more or less. During the operation, if the energy is exceeded or can not be reached up to 100%, click Auto-gain to make it the balance.
2 Reference: S-H method or D2 lamp method is selected. 3 Setup: Send all the parameters in Fig.4-16 to the main unit of the instrument. For example, Main
cathode lamp current, auxiliary cathode lamp current, negative voltage and D2 lamp current, etc.
4 Auto- balance: It is used to adjust the current of the reference beam and make the energy of Main
instrument will automatically seek the peak value position of the designated wavelength and the optimal lamp position. Simultaneously, the energy of Main should be at 100% more or less so as to make the negative high voltage of the gain being matched (Only for Models AAS-110A/110B/120A/120B).
6 Wavelength: Click Wavelength, the instrument will automatically find out the position around the
designated wavelength. Then click S and L of Fine wavelength to adjust the wavelength position, and click Up and Dn of Lamp position to find out the optimal lamp position. If the gain (negative high voltage) is too high or too low, input a proper gain value and click Setup, or click Auto-gain to - 57 -
Fig. 4-17
Fig. 4-18 The functions of the icons in the left tool bar are described as the following. On-line icon: If this icon is changed into gray, that shows it is connected with the main unit of the instrument. Otherwise the computer will remind you of no respond from the instrument. Confirm if the power supply of the instrument is switched on. Please try to test it again. Instrument Control icon: Click this icon to appear Fig.4-16,and adjust it properly. Baseline Stability icon: Click this icon to test the baseline stability of the instrument as shown in Fig.4-16. When all parameters such as wavelength, energy and negative voltage, etc are setup well, click this icon to appear the page as shown in Fig.4-19. Click Zero and then Start. Thus the instrument starts to test the baseline stability. The test result can be printed out by clicking Print after the test of the baseline stability. Settings of the Baseline Stability: Double click the page of Stability Test as shown in Fig.4-19 to appear the page as shown in Fig.4-20. In this page, user can adjust the parameters of time, maximum absorbance (setting the max range in the window of Fig.4-19) and monitoring absorbance value (the expected stability range of the instrument).
- 58 -
Fig. 4-19
Fig. 4-20
- 59 -
Measurement Parameters icon: When clicking this icon to make Read delay, the settings of Read time and Damp constant and modification will refer to Fig 4-6. Flame Condition icon: It shows the flame atomic absorption method is used.
Graphite Furnace Condition icon: It shows the graphite furnace atomic absorbance method is used. Click it to modify the conditions of the graphite Furnace, please refer to Fig.4-10. Project Information icon: Input the analytical project information, such as Project name and Analyst name. Dilution icon: Modify the information of sample dilution, such as Sample blank, Blank repeat times and Concentration unit as shown in Fig.4-21. Re-slope icon: Insert a re-slop at any time during the determination of the unknown samples. Please refer to the section 4.3.5 and Fig. 4-9. Next Project icon: If selecting multi-analytical methods in the analytical project design, when the first method is completed, click Next Project icon automatically to change it to the next project.
- 60 -
Fig. 4-21
4.11 Operations 4.11.1 When all the parameters such as the wavelength, energy and the negative high voltage are set well
in Instrument Alignment page for Models AAS-110A/120A/130A/110B/120B/130B, click Finish to show the page as shown in Fig.4-22.
Figure 4-22
- 61 -
Figure 4-23 4.11.2 Flame Method STD Working Curve and Unknown Sample Measurement
- 62 -
Fig. 4-24
Fig. 4-25 For example as standard series solutions of Cu: 1g/mL, 3g/mL and 5g/mL. The following operation steps are: Open the air-compressor and the acetylene cylinder. Ignite the flame. Then put the sampling capillary into the blank distilled water and click Zero key to make the zeroing adjustment. After zeroing, suck in the standard blank solutions in sequence: 1g/mL, 3g/mL, 5g/mL, and click Read in order. If the Absorbance value is beyond the Y coordinate range during reading, double click the page of Fig.4-23 to appear Graph Pane window as shown in Fig.4-24. Use the keyboard to input the corresponding modified value and the coordinate time. If observing the standard curve after completing the standard series
- 63 -
solutions, click the Calibrate tab in Fig. 4-23 to appear Fig.4-25. In Fig.4-25, the Mask key is used to mask one standard point, and thus improve the correlation coefficient. Its operation procedure is that select certain of standard point, which influences the curve fitting, and click Mask key. If user wants to get back that point, click Mask key again. Click the Measure tab to go on the measurement.
Fig. 4-26
Fig. 4-27 To modify a standard point or an unknown sample point during the analysis, click Data tab in the measuring page as shown in Fig.4-26. Select the standard point to be modified or the unknown sample point to be modified in the table, use the mouse to click it into blue color, and then click Remade key. The moment, the selected point has been deleted and return to measurement page to make the measurement again. In Fig.4-26, if clicking Delete key, the standard point or the unknown sample point and all data will be deleted at all. Detail key is used to show every standard point or every measuring value of the - 64 -
unknown sample point and calculate the average value and precision. The detailed information can be printed out by clicking Print key as shown in Fig.4-27.
4.11.3 Drafting of Standard Working Curve of Graphite Furnace and Unknown Sample Measurement (Only for Models AAS-110A/120A/130A)
The operations in the software between the graphite furnace method and the flame method are different on the Measure page as shown in Fig.4-28. The operations on the other pages are the same as the flame method, so please refer to the flame method. When the cooling water system, gas supply system and electric system are connected well and the instrument is running normally, inject the standard blank and standard series samples into the graphite tube of the graphite furnace, and then click Read key in order. If the Absorbance value is beyond the Y coordinate range during reading, double click the page of Fig.4-28 to appear Graph Pane window as shown in Fig.4-29.
- 65 -
Fig. 4-28
Fig. 4-29
1 Y-Axis: In Type list, if Customized is chosen, input a corresponding coordinate value at the Max.
If Auto- is chosen, the measuring page in the software will automatically adjust the Absorbance value according to its amount.
2 Show background: If select , that shows that BG value of the D2 lamp or S-H deduction
measurement.
4 Overlapped: Make the standard sample curves and the unknown sample curves overlapped.
- 66 -
5 Signal: It is used to display the graphs of all samples. Time average is used for the flame method, a
straight line is displayed. The peak shape of the collecting sample is displayed for the graphite furnace method as shown in Fig 4-30.
6 Result: The final result is obtained for the determination of the unknown samples as shown in Fig.
4-31. If the existed format is not required by the user, you can edit the format by yourself. Click the Excel key to make the edit, but the origin format cant be overwritten by the new edited format.
- 67 -
Fig. 4-30
Fig. 4-31
The selection of the measurement condition refers to the Fig.4.6. Select the standard addition method in Measurement condition page as show in Figure 4-6. In the Working Curve of Fig.4-7, input 0 as S1, and input the unequal amount of the standard solutions as S2, S3 and S4. Since the contents of the co-existed substances are all quit same in this group solution, thus the standard curve obtained should be the straight line without passing through the original point as shown in Fig.4-32. The concentration of the sample to be determined is shown in Fig.4-33. The standard addition method can eliminate the matrix interference and obtain the more accurate results. But it cannot eliminate the background absorption interference.
Fig. 4-32
Fig. 4-33
4.11.5 Print
Select File>>Print from the menu to print the working curve, data table, signal graphs and results. - 69 -
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temperature can be reached up to 3200OC. When the turbulent flow burner was adopted, the flame is very unstable. When the pre-mixed burner was adopted, the flashback is easily occurred because of the bad design of the burner, which caused that the burning speed is too fast during poor flame combustion. Hence, their design was not generalized. Mr. Kirkbright researched the tri-slit burner oxygen shielded air-acetylene flame to avoid the flashback. But the flame temperature is only 2600OC and there is much noise. Its performance is not as good as the N2O-acetylene flame. The key of improving the AAS sensitivity and decreasing the chemical interference is to increase the flame temperature. While the key of the increasing flame temperature is to increase the content of oxygen in the assistant combustion gas and to randomly adjust the flow of all gas components. The enriched oxygen air-acetylene flame AAS is a new type of patent technology (patent No. 92101560.7). In this method, add the pure oxygen into the air to be concentrated air, and then mix them with the acetylene. Accurately control the flow of all gases respectively by the flow meter to obtain the best flame status for various elements so as to obtain the optimal atomization efficiency. It is a new type of atomic absorption spectroscopy with high temperature, easy to operate, low cost, nontoxic and high sensitivity, which is used in many fields for the trace analysis. The flame temperature can be controlled by adjusting the flow of the oxygen and the acetylene, so this flame method can be used for various elements. For the first-class elements, use the air-acetylene flame without the oxygen. For the second-class elements, use the enriched oxygen air- acetylene flame and the sensitivity will be improved far more than that of the air-acetylene flame or the N2O-acetylene flame. For the third-class elements, the sensitivity of the enriched oxygen air-acetylene flame is almost the same as that of the N2O-acetylene flame. Since the high temperature burns so low under the enriched condition, so the flashback hardly occurs, it is safety. When the lean flame is used, the combustion speed is fast, and the carbon will be accumulated on the edge of burner slot. So when the enriched oxygen air-acetylene flame is used, normally it should be made under the enriched combustion or gentle enriched combustion (reducing).
5.2.1 Connect the pipes of the air, the acetylene and the oxygen correctly according to the requirements of the installation mentioned in this manual. 5.2.2 Power on the instrument and start the communication between instrument and computer. Select the flame atomic absorption method. 5.2.3 Turn the oxygen knob on the left panel clockwise to the end. That means the oxygen flow is zero. Check this position before the ignition. 5.2.4 Power on the air compressor and adjust the output pressure to 0.3MPa. Open the acetylene cylinder and adjust the output pressure to 0.5~1.0MPa. Open the oxygen cylinder and adjust the output pressure to 0.1MPa. 5.2.5 Insert the oxygen key into the switch keyhole and turn it to make the arrow to On position, and the indicator is on. 5.2.6 Adjust the acetylene knob and make its flow being 1~2L/min. Press the ignition button, and ignite the air-acetylene flame. Go on increasing the acetylene flow to 6~7L/min, and now the flame color becomes red. (The acetylene flow should be less than 10L/min.) 5.2.7 Adjust the oxygen knob and increase the oxygen flow slowly to 3~4L/min. Now the flame color is baby blue. In this condition, the analysis can be made. 5.2.8 Analyzing operations are the same as the air-acetylene flame method. 5.2.9 During the determination, if the sensitivity is lower, firstly increase the acetylene and then the oxygen, adjust the flows of the acetylene and the oxygen repeatedly until the flame temperature meet the analyzing requirement. Note: the oxygen flow must be less than 70% of the acetylene flow so as to avoid the flashback. 5.2.10 Close operations: Firstly decrease the oxygen flow to 2L/min slowly, and then decrease the acetylene flow to 4L/min. Note: the sequence must not be reversed. 5.2.11 Go on decreasing the oxygen flow to the zero. Turn off the oxygen switch. And then decrease the acetylene flow to the zero. At last close the main switch of the cylinders and power off the air compressor. Note: Customer should make the analysis following the above steps. If the operations are correct, the flashback will not be occurred. Once wrong operation occurs, the protection device in the instrument will avoid the occurrence of accident. In an emergency, press the ignition button to shut off the flame directly. - 73 -
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hollow cathode lamps with different elements have the different life time. HCLs lifetime also depends on the working current. The replacement of HCL is very simple. Pull up the lamp from the adapter and plug the hollow cathode lamp to be used into its adapter and place it into the lamp turret. There are six lamp adapters for Models AAS-110A/110B/120A/120B (AAS-130A/130B has four lamp adapters). All of the lamps can be simultaneously inserted or insert any of the lamps required. The light spot of hollow cathode lamp is generally auto-adjusted when the wavelength is scanned. If the error is very large, adjust it as the following: (1) Place the HCL into the No.1 lamp position and set the lamp current as 5mA. A red light spot will occur on the right wall of the atomization chamber. (2) There are four screws on the No.2 lamp position. Keep two screws located at the middle immobile, and loose the other two screws located outside. Rotate the lamp turret and make the light spot in the middle of the lens and then screw the two screws.
Tube Voltage Drop: 70VDC Filament Voltage: 10VAC Filament Current: 0.5A Glow Voltage: more than 200VDC
2) The D2 lamp used in this instrument has four lead-in wires. The red one is anode lead-in wire. The two black wires are filament lead-in wires and the yellow one is auxiliary electrode lead-in wire. Do not touch the window of D2 lamp by hands. 3) The window of D2 lamp should be aimed at the half-transmission-half-reflection lens during the installation. 4) The light spot of D2 lamp is very small, so carefully makes the alignment being light after the replacement. If the light spot position is not adjusted well, it will influence the energy output of D2 lamp and the light spot overlapping with HCL, and the background correction will be also affected. - 76 -
5) Adjustment method: (1) Power on D2 lamp and set the current as about 60mA. Select the slit to be 0.4nm. Power on Cd HCL with 3mA; (2) Place a piece of paper in the middle of the burner and observe the light spot of D2 lamp and Cd HCL on the paper. Adjust the top end of D2 lamp holder and side of the screws until the two light spots are overlapped. (3) After automatically seeking the peaks, adjust the energy of D2 lamp to make the BG energy to the maximum. Now the replacement and adjustment of D2 lamp is over. 6) Ignite the D2 lamp and adjust its position. Be careful that the D2 lamp is very hot!
(3) If the HCL is broken, the cathode substance is exposed. And some element materials are harmful to human body, so they should be processed according to standard laboratory method. 2) D2 lamp The lifetime of D2 lamp will be shorten if it is frequently powered on and off. (2) Do not touch the light passing window with fingers. After the replacement, clean the window with the absorbent cotton dipped with alcohol-ether mixture solution, and then power on the D2 lamp.
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atomization chamber and the burner. If the samples concentration is very high or the samples are turbid solutions, do clean them after the analysis every day. If the samples are organic solutions or high concentration such as, Cu, Ag or Hg solutions, do clean them just after the analysis, because the unstable acetylide will be generated, which is detonatable. The clean method of the organic solutions is: firstly spray the organic solution with sample mutually dissolved for about 5 minutes; then spray acetone for about 5 minutes; and then spray 1%HNO3 solution for about 5 minutes; at last spray de-ionized water for about 5 minutes. 2) Maintenance of Nebulizer (1) If the front end of the capillary in the nebulizer is blocked up, do not poke it with metal silk, which will damage the glass parts. The methods of removing the stem are that blow the capillary in the negative direction or pump it inversely. For the organic stem, take off the nebulizer from its holder and dip its front in the potassium dichromate solution to dissolve the block. (2) After a long time use, if the sediment occurs in the nozzle of the nebulizer, the spraying quantity will be decreased and the sensitivity will be affected. In this instance, take off the nebulizer and clean the nozzle. (3) If the plastic absorbing capillary is bent to be not available, dip it up in the hot water. Then make it straight and cool it down. 3) Maintenance of Atomization Chamber Take off the burner head, and pour 50mL de-ionized water into the upper neck of the atomization chamber. Let the water flow out through the waste liquid pipe. Repeat this step for several times. If the atomization chamber is still not clean, dismount it and clean it with surface-active agent solution, and then wash it with the de-ionized water. If the instrument will be not used for a period of time, wipe all of solution drops inside of the atomization chamber. (1) Do not jerk or wrest the atomization chamber and its holder hardly. (2) Mount or dismount the atomization chamber holder carefully. Do not throw it. (3) Do not scratch the atomization chamber inner with metal or other hard object. (4) The connection between the atomization chamber neck and the burner head is sealed by O-rings. When dismounting the burner head, please turn it slowly and pull it out in the direction of the atomization chamber neck. Do not force it strongly to avoid the damage the neck. 4) Maintenance of Burner The flame from the long slot of the burner should be steady. If not and the flame varies randomly for a long - 79 -
time, there should be the sediment in the slot. The clean method is: blow it with the air compressor and scratch the slot sides carefully with single side blade. Do not damage the slot sides. Anther method is: clean it with corrosive soapsuds. 6.3.3.2 Graphite Furnace System Maintenance of the graphite furnace system mainly is to clean the graphite furnace, including the graphite tube, the graphite cone and the quartz windows. There is no sample pollution in graphite furnace analysis generally. The cleaning intervals will be decided according to the analytical conditions. Details about the maintenance of the graphite furnace system refer to its own operation manual.
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6.4.2 Main Board (PC1) The schematic diagram of the main control PC Board is shown in the following Fig. In Main Board figure: 1)Cable plug (1) of HCL, among them, pin 1 is connected to the earth; the rest sic pins are connected with short circuit and connected with the lamp voltage of 400-450V. 2)HCL plug (2). Pin8 to lamp1; Pin7 to lamp2; Pin6 to lamp3; Pin5 to lamp4; Pin4 to lamp5; Pin3 to lamp6 of controlling signal. Pin2 to lamp 5 and Pin1 to the auxiliary current of lamp6. 3)Control signal of scan motor. 4)Control signal of lamp align motor.
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Main Board Figure 5)Control signal of slot motor. 6)Transformer socket, AC15V. Supply for +17V voltage regulator. 7)Sampling signal of hydride generator or online enrichment. 8)Optical couplers sockets respectively connect with lamp changeover location plate, scan location plate and slot location plate. 9)Connect to the communication plug-in of the graphite furnace system. 10)Connect to the computer. 11)GND(connection to ground). 12)Control plug-in of HV module. Pin1 to +15V; Pin2 to the yellow line of HV module, Pin2s voltage varies in the range of 0~5V. (1V corresponds to the output of 200V HV and 2.5V to the output of 500V HV) 13)Transformer socket. Pin1 and Pin2 to AC9V; Pin3 and Pin4 to AC17V; Pin5 and Pin6 to AC17V, respectively supply for the voltage regulator circuits of +5V, +15V and -15V. 14)Transformer socket. Pin1 and Pin2 to AC160V. Supply for the voltage regulator Circuit of +200V. 15)D2 lamp socket. Pin1 to yellow line; Pin2 to red line; Pin3 and Pin4 to black lines. The voltage of Pin2 is 200V. The voltage between Pin2 and Pin1 is 70V. The AC voltage between Pin3 and Pin4 is 10V. - 82 .
16)Transformer socket. Pin1 and Pin2 to AC10V. 17)Transformer socket. Pin1 and Pin2 to AC300V. 1TP1 is +17V for motor. 1TP8 is +15V. 1TP9 is -15V. 1TP10 is +5V. 1TP11 is +400V for HCLs. 1TP21 is GND. One end of 1R19 is 200V for D2 lamp as shown in Figure. HV Module Total four lines. Red and white lines to HV control socket; black line to GND; both ends of shielded wire is HV output. Note: All the above DC voltages are relative to GND and all of the voltage values are approximate values.
1Electrical Magnet Valve plug seat. Pin6 connects to lock of switch; Pin1 and Pin3 connect to ignition electrical magnet valve; Pin2 and Pin4 connect to acetylene electrical magnet valve; Pin5 connects to oxygen electrical magnet valve, the other end of oxygen valve connects to lock of switch.
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2)Ignition switch plug seat. Pin1and Pin2 connect to the constant open contact points of ignition switch. 3)Plug seat of flame monitor board. Voltage of Pin1 is +5V; Pin2 is monitoring voltage (<+5V); Pin3 connects to GND. 4) Pin1 and Pin 2 connect to alarm light-emitting diode; Pin 1 connects to positive; Pin2 connect to negative. 5)Igniter socket. Pin1 connect to positive pole of ignition module; Pin2 to GND. When igniting, voltage between Pin1 and Pin2 is about +2.5V when ignition. 6)Transformer plug: Voltage of Pin1 and Pin2 are AC9V; Voltage of Pin3 and Pin4 are AC27V. 7)--- Transformer plug. Voltage of Pin3 and Pin4 are AC8V. 5TP1 is +21V. 5TP2 is +5V. 5TPO is GND (0V) Gas control board is easily affected by the environmental changes, including odor and light, so the ignition failure or the alarm may be occurred sometime. The adjustment may be required as follows: (1) When the output pressure of the air compressor is 0.18MPa, adjust 5RP1 to make the voltages of 5TP7 and 5TP8 being the same. (2) Adjust 5RP3 to make the voltage value of 5TP6 being 2.5V. (3) Adjust 5RP2 to make the voltage value of 5TP3 0.2V lower than that of 5TP4. Note: All the above mentioned voltage values are relative to GND.
See Signal Amplifier Board: 1)Network connector. To the output signal of PMT. 2)Pre-amplifier. Transfer the current signal of PMT to the voltage signal. 2RP1Zero adjustment potentiometer. When the voltage is zero or the lamp current is zero, the absorbance value of the instrument should be zero. If not, adjust this potentiometer to be the Zero. 2RP9 signal adjustment potentiometer of hollow cathode lamp. 2RP4Background signal adjustment potentiometer.
5) Vertical motor socket. Pin1 Pin4 respectively to lead-in wires of red, green, yellow and blue. 6) Horizontal motor socket: Pin1 Pin4 respectively to lead-in wires of red, green, yellow and blue. 7) Power supply socket: Pin 1 and pin2 to ~18V; Pin 3 and pin4 is ~18V; Pin 5 to GND.
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Fig. 6-1 4) If there is no same graphic appearing shown as Fig. 6-1 after scanning, or three peaks are not appeared at the same time, on this occasion, the scanning range is required to be modified. Quit this scanning page and again click Wavelength Scan key to enter into Wavelength Scan page, modify the scanning range. The Starting wavelength value is changed into 310.0nm (330.0nm). The End wavelength value is changed into 320nm (or 340nm), and so on. Re-input Gain value under special conditions. In general, The re-setting range is normally in the range of 10nm, change it until the quite same graphic appeared is as same as the graphic shape as shown in Fig. 6-1. Note: In normal case, seek the wavelength range between 300~350nm. 5) Return the program to the page of Fig.4-1, successively click Help(H) and Instrument parameter setting to enter the page of Fig. 6-2. X1 and X2 obtained will be substituted into the formula: 1 = X1 324.7 and2 = X2 - 327.4. 6) Input the wavelength value of 324.7nm, and the deviation value is1. Input the wavelength value of 327.4nm, and the deviation value is2. Click Calculate and OK. The moment, the wavelength parameter is re-confirmed. If the parameter is not loosen, the re-confirmation is required. Normally the wavelength transition problem is solved all.
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Fig. 6-2 6.5.2.2 Adjustment of Wavelength Nonlinearity. If re-confirming the wavelength parameter of the instrument, the wavelength of the instrument is not linearity or the wavelength of some element can not be found at all, so please follow the following adjustment procedures: 1) When the wavelength of 324.7nm is confirmed, ignite the Hg hollow cathode lamp (lamp current is 3mA). After entering into the optical path, scan the wavelengths nearby of 253.7nm (gain 200V more or less), 546.1nm (gain about 300V) and 871.6nm (gain about 400V), thus judge if the wavelength change of the system is linear or not, that is: value should be less than 0.25nm. 2) If the three wavelengths are over deviation, the program will be returned to the page of Fig.4-1, successively click Help (H) and Instrument parameter setting to enter into the page of Fig 6-2, respectively input the three wavelength values (253.7nm, 546.1nm and 871.6nm) and three values (1 23) into the frames of the wavelength and the deviation. Click Calculate and OK, the moment, the wavelength calibration of the whole system is completed. Note: 1) The procedures above-mentioned sometimes are required to be done repeatedly. 2) User can not change the instrument parameters without the authorization. If the instrument parameters must be modified, please contact with your local distributor (firstly take notes for the parameters, and then modify it again. Refer to the section 6.6.4).
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6.5.3 Common Troubleshooting Analysis 6.5.3.1 Power Indicator is not lit Reasons
(1) Power lead-in wire is cut off or bad contact. (2) Fuse is damaged or fuse adapter dropout (3) Power open circuit. (4) Signal input cable loose or poor contact.
Solution
Check it with universal meter. Resistance between power live wire and cabinet > 20M. After closing the power switch, the resistance between power cables should be 10.
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tube(1794) is broken down; if all lamps do so, take them out and check the 15V, +5V on measuring main board.
When enlarge the lamp current, the tails of anode and cathode in the lamp tube has light radiation.
The electric shield performance between anode and cathode is bad, so breakdown and discharge occur due to high lamp current.
6.5.3.4 Display Please power on the main unit of the instrument on the screen when the instrument is making the self-check.
(1) Check if the instrument has been powered on. (2) Check if the communication cable between the instrument and the computer is connected well. (3) Check if the cable plug of the computer is connected in the right position. One end of the main unit should be plugged in Computer socket. One end of the computer should be plugged in COM2 or the - 90 -
only COM of computer. (4) Setting of the series interface is not correct, close it and enter the program again, click Help(H) Instrument Parameter set to appear Fig.6-2, modify the communication interface COM2 (or COM1) in the page. 6.5.3.5 Check if +5VDC voltage exists on the main board and the computer socket on the main board is contacted well.
Note: Ensure the negative high voltage is switched off before opening the monochromator. Never touch the surfaces of the optical parts when the monochromator is opened. 6.5.3.7 Sudden lamp off and position change.
(1) If the power supply is suddenly off without knowing, only power off the main unit of the instrument and then power it on again. (2) If the power cable is not connected well, switch off the main unit of the instrument and pull out both ends of the power cable, use a clipper to slightly rotate the three contacting pins on the three phase socket of the main unit as so to make the good contact. Hollow cathode lamp itself is abnormal.
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Re-ignite for more times and remove the air out from the pipes.
After ignition for a while, the flame is off and alarm. Igniter can not ignite the flame. Alarm lamp is on and alarm sound is continually sent. Alarm sound is short like Di, Di . Alarm sound is longer but has pause. 6.5.3.9 Energy is too low. Reasons
Acetylene leakage exists in the piping. Igniting needle is oxidized for a long time use. Gas sensor circuit alarm.
Check the piping and connectors with soap water. Clean the igniting needle with sand paper. Adjust 5RP3 according to the section 6.5.3.
Solution Replace a new lamp. Re-adjust the optical system and make the light spot just aimed at the incidence slit.
Clean the lens with alcohol-ether mixture (ratio 1:3) or replace it.
Clean the optical parts or replace them. See the section 6.4.2.
(1) Stop spraying when the instrument is unstable. If the instrument becomes stable, reasons may be the
following. Reasons Impact bead position is changed. Solution Shut off the flame and re-adjust it. Slightly rotate the impact bead to make the bent neck locating at downward; slightly move the impact bead forth and back to make the fog
uniformly forward when spraying. Capillary tube is blocked. Blow it with air compressor or clean it with clean liquid or replace a new one. Waste tube is blocked Nebulizing chamber is polluted seriously. Clean it or replace a new one. Wash it with acetone, HNO3 and de-ionized water. Strong emission of solution compounds occurs in the flame. Remove these components with chemical method.
(2) Stop spaying if the instrument is still unstable, shut off the flame. If the instrument becomes stable,
the reasons may be the following. Reasons Combustion gas is not pure. Ratio of combustion gas is too big and flame emission is large. Nozzle is polluted seriously. Flame absorption is big in short-wave zone. Replace a new one. Use background corrector. Verify it with Cu or Mg lamp. Burner head is blocked. Burner position in optical path is not correct. See the section 6.4.3.1. Adjust the burner up or down, front or back and its turning angle, referring to the sections of 3.3.4 and 3.3.5 Air is unstable. Replace a new air flowmeter. Purify it. Use smaller band pass (narrow slit). Solution
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(3) If shut off the flame and the instrument is still unstable, the reasons may be the following.
Lamp Status Bad lamp Emission intensity is low and negative HV is set too high. Increase the lamp current. Widen the slit. Replace a new lamp. Lamp emission is unstable and lamp background is large. Good lamp There is too much water in pipes. Waste liquid is full and pour it out in time. There is water in gas piping or air flow meter. Pull out the air out pipe on the back of gas control, open the air compressor, use hand to block the gas nozzle and then loose it again, makes the air to drain off water. Combustion gas is unstable. There may be gas leakage in output pipes of acetylene cylinder. Or C2H2 flowmeter is bad. Replace a new one. Wavelength is not correct. Re-adjust the parameters referring to the section 6.6.2. Troubles in electronic system. Voltage of electric network changes large. Ground wire is not connected well. Connect it to ground directly with copper board. HV module output is unstable. Some components are not contacted well in the circuit. Replace the HV module. Shut off the instrument and check them carefully. Use the voltage regulator. Replace a new lamp. Reasons Solution
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Some components are damaged in the circuit. Hard magnetic field or high frequency interference.
Repaired by manufacture.
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Solution Verify it with standard solutions and process the samples to remove the interference.
Standard solution is wrongly prepared or is polluted. Sample concentration is decreased because of container absorption. Blank solution is polluted.
Verify it with other element standard solution and re-prepare it. Verify it with other element solution and re-prepare it. Prepare new blank solution.
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Burner is not pre-heated enough. Capillary is blocked up or attacked. Waste liquid flow is not good enough. Gas supply system is unstable.
Prolong the pre-heating time for 3~5 min. Clean it or replace it. Clean it.. Check if there is water in pipes or if the gas source is stable.
Note: Once flashback occurs, check if the explosion proof film is damaged. Plug the intact explosion proof plug into the back of the nebulizing chamber. Also check if the nebulizer and burner are damaged. If all are ready, may ignite it again.
Reasons Lamp lifetime is over Glow voltage increases after long time use. Trouble in power supply circuit. Replace a new one.
Solution
Replace a new one when it cant glow. Measure the voltages of the four wires of D2 lamp. Voltage of red wire to Earth is about DC200V, and voltage between two black wires is about AC10V.
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Atomization temperature is too high. Background value > 1.0A(D2 lamp background correction method); Background value > 1.8A (S-H method).
Select proper atomization conditions Process the samples and decrease the background value properly.
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After the computer is automatically installed, appear the following window, click Finish.
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Appear the following window, click OK. When the installation of the software is completed, there appears a shortcut icon AAS-110 on desktop.
Note: There is only one program installed in the disks. Before next installation, delete the previous software, otherwise it can not work in normal. 6.5.4.3 Input parameters method Each instrument has its own parameters. After installation of the software, parameters marked on the software disk case are required to be input into the computer. Click StartRuninput Regeditclick click OK, open the click editor. Double click click
HKEY-CURRENT-USERdouble
softwaredouble - 102 -
BRAICdouble
BRAICdouble click Generaldouble click computer display parameters pagedouble click Optical Origininput parametersOKdouble click Optical Ratioinput the parameters OK. After closing the register editor, the instrument can run in normal. 6.5.4.4 Find parameters If the software is required to be installed or the parameters is required to be modified, please record the parameters for later using. Click StartRuninput Regeditclick click OK, open the click editor. Double click click
HKEY-CURRENT-USERdouble
softwaredouble
BRAICdouble
BRAICdouble click Generaldouble click computer display parameters pagedouble click Optical Originrecord the parametersOKdouble click Optical Ratiorecord the
parametersOK.
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