Sunteți pe pagina 1din 104

Operation Manual for

AAS-100 SERIES ATOMIC ABSORPTION SPECTROPHOTOMETER

PLEASE READ THIS MANUAL CAREFULLY BEFORE OPERATION


3, Hagavish st. Israel 58817 Tel: 972 3 5595252, Fax: 972 3 5594529 mrc@mrclab.com

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 2 Environment Requirements ........................................................... 22


2.1 Working Environment .................................................................................................22 2.2 Transportation and storage condition........................................................................22 2.3 Laboratory Conditions for Safety Operation ............................................................22 2.4 Other Requirements.....................................................................................................25

Chapter 3 Installation..................................................................................... 27
3.1 Acceptable goods ..........................................................................................................27 3.2 Unpacking .....................................................................................................................27 3.3 Installation ....................................................................................................................27 3.4 Acceptance Inspection..................................................................................................38

Chapter 4

Software Operation ................................................................... 43

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
-1-

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

Enriched Oxygen Air-Acetylene Flame .................................... 71

5.1 Introduction of enriched oxygen air-acetylene flame................................................71 5.2 Operation of enriched oxygen air-acetylene flame....................................................72

Chapter 6 Maintenance and Service............................................................. 75


6.1 Attention Points for Maintenance...............................................................................75 6.2 Replacements and Adjustments of Components and Parts......................................75 6.3 Daily Maintenance........................................................................................................77 6.4 Circuit Schematic and Function Description.............................................................80 6.5 Trouble Shooting ..........................................................................................................86

-2-

Important:

Please Read the Following Carefully Before Operating the Instrument!!!


POINTS FOR ATTENTION TO FLAME OPERATION
1. Make sure that the gas lines are all correctly connected. 2. Be sure that the water seal has been well formed before ignition. 3. Before ignition, be sure that the O2 and C2H2 flow have been turned clockwise to minimum. 4. Ignition procedure: a. Adjust the outlet pressure of the air compressor to 0.3Mpa more. ignition button. b. Press down the

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.

-3-

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

-4-

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.

-5-

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.

-6-

Safety 2 2.1. Characteristics of acetylene


2.1.1 Physical and chemical characteristics Appearance and olfaction: Colorless and liquefied solution gas. Flavor: pure flavorless, but the acetylene has been sold on the market with some special garlic flavor. Molecular quantity: 26.04 Molecular formula: C2 H2 Boiling point: -75 Melting Point: -82.2 Flash Point: -18 Explosion bounds: low explosion limited: -2.55%, up explosion limited: -81% Self-combustion temperature: 305 Density of vaporization (air=1, 20): 1atm: 0.906 Density of the liquid: (-82), 1atm, 0.621 Vapor pressure: (21.1), 4.375Mpa Specific volume: (20), 1atm.....................9.1710-4m3/g. Solubility in acetone: 15, 1atm, 20m3/m3 15, 12atm, 240m3/m3 2.1.2 Generation of the acetylene Hydrogen atom on the triple bond is weak acid. (PKa=25), it can be replaced by metal element, and generated to be the acetylene.

The reaction generating acetylene Ag or Acetylene Cu is very sensitivity, so the acetylene and the end-base

-7-

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.

2.2. Safety requirement for acetylene gas


Users should know and understand something about the configuration of cylinder and the characteristics of the acetylene. The following basic safety rules are described, such as: storage, operation and using guide of the acetylene cylinder. 2.2.1 Configuration and requirement of the steel cylinder.

(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

-8-

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

Storage, transportation and usage of the acetylene cylinder Storage:

(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

-9-

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.

2.3.4 Engineering Control:


Provide natural and explosion-proof ventilation conditions to keep the concentration in the room less than the explosion limit. 2.3.4.1 Treatment of the waste gas. (1) Unused and residual gases should be returned to the vendor. Dont handle with it by yourself. (2) If there are proper combustion devices on the site, burn off the residual gas in the system to avoid polluting the environment. 2.3.4.2 Safety requirement when using the air-acetylene flame operation or analyzing samples such as copper, mercury and silver. According to the above description for the chemical and physical characteristics, copper, mercury and silver will be easily generated to be metal acetylene compound when meeting the acetylene. When it is heated and shocked, it might be decomposed and exploded. Therefore, the following operating regulations must be followed when the above three elements are determined with the air-acetylene flame operation. (1) The connection piping from the outside of the acetylene source to the instrument in the room can never use the copper, silver and mercury or the alloy materials. (2) When completing the determination with the air-acetylene operation per day, turn off the cylinder valve under igniting state. Let the residual gas inside of the piping burn off as much as possible, the flame is naturally off. Afterwards, turn off the voltage regulator, at last, switch off the air-compressor. (3) Before the determination by the air-acetylene flame operation, firstly take off the cover of the instrument, power on the ventilation device installed above the instrument for about 20 minutes so as to avoid the explosion caused by the residual gases in the room. - 11 -

(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.

2.3.5. Proposal of the accident


2.3.5.1 Handle with being on fire: The acetylene is flammable gas, special carefully for flame off, the acetylene sources must be cut off. It is very important to avoid the acetylene gas accumulating in a narrow space, because the fire and explosion can be again caused. The fusible metal plug on the top and the base of the cylinder can be melt down at 100. In this case, the fusible metal plug is melt, the fire from it can be sprayed to about 4~6 meters away. (1) If one cylinder got fire and will link to the other cylinders, the moment, spray water to the cylinders to get down their temperatures. It is very important to avoid their fusible metal plug being melt down. (2) If all cylinders got fire, people must get away from the area as soon as possible and leave the experienced person to take in charge of it. Turn off the valve to cut off the acetylene if it is possible, and then try to get off the combustion materials. Burn off the residual gas if stopping the leakage impossible to avoid the gas accumulation to cause the mixture gases burning again. (3) Suitable fire-extinguish agent: Chemical drying powder, carbon dioxide and water should be used. Never put out the fire unless the valve of the cylinder is closed. (4) Special equipment for firemen: Fire-proof dresses must be put on the fire-men and carry positive type - 12 -

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.

- 13 -

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.

Fig. 1-1 AAS-100 series AAS 1.2 Main Features


1.2.1 High automation AAS-100 series AAS including AAS-110A/110B/120A/120B/130A/130B can provide many automatic functions, such as: auto-wavelength setting, auto-wavelength scan, auto-slit exchange, auto-peak-picking (except for 130A/130B), and auto-adjust the light (except for 130A/130B). Flame out protection and alarm, air pressure relief protection and alarm, combustion gas leakage protection and alarm, etc are also provided. Air-acetylene flame method can be used for models AAS-110B/120B/130B. Air-acetylene flame method and graphite furnace method can be used for models AAS-110A/120A/130A. They adopt incorporated atomizer design, which means that the flame atomizer and the graphite furnace atomizer can be switched randomly when changing analysis method. Two background correction methods are used such as: Deuterium lamp background correction method and self-absorption background correction (or S-H method). Models AAS-130A/130B can only provide with D2 lamp background correction technique. - 14 -

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.

- 15 -

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

Fig. 1-2 Block diagram


- 16 -

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 -

1.5 Performance Characteristics


1.5.1 Wavelength Range and Wavelength Accuracy Wavelength Range: Wavelength Accuracy: 1.5.2 Resolution The double lines of 279.5nm and 279.8nm Mn can be resolved and the energy value of the wave bottom between two spectral lines is less than 40% of energy of 279.5nm. 1.5.3 Characteristic Concentration (CC) (or Characteristic Quantity), Detection Limit (DL) and Precision 1.5.3.1 CC, D.L. and R.S.D of Air-acetylene Flame Method: Element: Cu, Wavelength: 324.7nm CC0.04g/mL/1%,; D.L.0.007g/mL, Precision 1% 1.5.3.2 Characteristic concentration of enrich-ed-oxygen-air acetylene flame method: NOTE: AAS-120A/120B/130A/130B are not available Element: Ba, Wavelength: 553.6nm; Enrich-ed-oxygen-air acetylene flame CC is less than 0.22g/ml/1% 1.5.3.3 Characteristic Quantity and Precision of Graphite Furnace Method: NOTE: AAS-110B/120B/130B models are not available. Element: Cd, Wavelength: 228.8nm CQ: 110-12g, Precision: 5% 1.5.4 Stability of Baseline Zero Drift of Static Base Line in 30min is less than 0.005Abs; Zero Drift of Dynamic Base Line in 10min is less than.006Abs. 1.5.5 Background (BG) Correction Ability NOTE: AAS-110B/120B/130B models are not available. D2 lamp method: When the background absorption is near to 1Abs, the background correction ability is more than 30 times. S-H method: Model AAS-130A is not available. When the background absorption is near to 1.8Abs, the background correction ability is more than 30 times. 190900nm 0.25nm

- 18 -

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

1.6 Models, Specifications and Standard Configuration


Table1: Specifications of different models, which are manufactured by our company. Model Configuration Main unit, Computer, printer, Air compressor, Incorporated AAS-110A atomizer, Power supply of Photofurnace Main unit, Computer, printer, Air compressor, Incorporated AAS-120A atomizer, Power supply of Photo-Control furnace Main unit, Computer, printer, Air compressor, Incorporated AAS-130A atomizer, Power supply of Photo-Control furnace Main unit, Computer, printer, Air AAS-110B compressor, flame Six lamps of auto-changeover, auto-peak picking, auto-wavelength scan, air-acetylene flame, Graphite Four lamps of auto-changeover, wavelength setting, auto-wavelength scan, incorporated atomizer, Graphite Control Graphite Specification Six lamps of auto-changeover, auto-peak picking, auto-wavelength scan, incorporated atomizer,

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

background correction, S-H back ground correction.

air-acetylene flame, D2 lamp back ground correction.

atomizer.

enriched-oxygen air-acetylene flame, flame emission, D2 lamp background correction, S-H background correction.

Main unit, Computer, printer, AAS-120B Air compressor, flame

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.

atomizer. 1.6.1 Specifications 1.6.1.1 Wavelength Range: 190900nm

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

1.6.2 Standard Configuration


Main unit Computer Printer Air compressor *Graphite Furnace System #Standard Accessories Operation Manual *Only provided by AAS-110A/120A/130A. #Note: Includes some accessories, tools and fluid pipes. 1set 1set 1set 1set 1kit 1kit 1copy

1.7 Electronic Safety classification


1.7.1 Shock proof type : class device. 1.7.2 Shock proof grade: B type device. 1.7.3 Harmful fluid proof grade: Common type. 1.7.4 Working Mode: Intermittent operation.

- 21 -

Chapter 2 Environment Requirements


2.1 Working Environment
2.1.1 Environmental Temperature: +10OC+30 OC 2.1.2 Relative Humidity Range: 30%85% 2.1.3 height above sea level range0-4000m. 2.1.4. No strong magnetic field interference. 2.1.5. No shake in the room. 2.1.6. Clean, dry, no dust and no corrosive gas in the room. 2.1.7. No fire, no electric heating or spark generating equipment. 2.1.8. Lightning rod should be installed on the lab top.

2.2 Transportation and storage condition


Rain, strong shinning, or hard shock should be avoided during the transportation. The instrument should be kept well with the original packing box in the room before the installation. The environmental conditions for the transportation and storage should be as follows: 2.2.1 Environmental temperature range: -40~55 OC; 2.2.2 Relative humidity range: 93%.

2.3 Laboratory Conditions for Safety Operation


The requirements all mentioned in this section must be met before the instrument is installed and adjusted.

2.3.1 Power Supply Requirements


2.3.1.1 Voltage, Frequency and Power of power supply
1 Main unit , Computer and Printer: AC220V22V, 50Hz, totally power 500VA. 2 Air Compressor: AC220V22V, single phase AC, 50Hz, 240VA. 3 Graphite Furnace Power Supply: AC380V, 50Hz, 6kVA. 4 Auto-sampler of graphite furnace: Single phase A.C.220V 22V, 50Hz,

2.3.2 Power Supply Connections


2.3.2.1 The power supplies of main unit, computer and printer should be to use the stabilizer device. The laboratory switchboard and the socket specifications are shown in Fig.2-1. 2.3.2.2 Separate the supply phase lines of this instrument from that of those devices with high power or strong electromagnet interference. - 22 -

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.

Fig.2-1 Laboratory Switchboard and Socket Specifications

2.3.2 Requirements of Gas Supply


2.3.2.1 Necessary Gases
1 Compressed Air: The outlet pressure of the air compressor should be adjusted to 0.3MPa. It is

necessary for the flame operation.


2 Acetylene gas: The cylinder filled with the acetylene gas is used with a specialized decompress

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

- 23 -

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.

2.3.3 Cooling Water Requirements


Cooling water is used for the graphite furnace operation. 2.3.3.1 Tap water with flux of 1.9L/min or water chiller is available for use. 2.3.3.2 Water pressure should be up to 0.15MPa, the inlet temperature can not be higher than 25. 2.3.3.3 The jointer with 8mm (ID) plastic tube should be mounted at the outlet port of the water supply

2.3.4 Ventilation Requirements


2.3.4.1 When analyzing samples with atomic absorption spectrometer, many gaseous matters will be created, so it is the necessary to install the ventilation device in the laboratory. 2.3.4.2 The exhausted outlet should be mounted above the atomizer. The installation ventilation device refers to Fig.2-2. 2.3.4.3 The wind flow volume is favorable while a paper is just absorbed by the back of the extraction fan. Neither too large nor too small is advisable. The former will affect the stability of the flame, and the latter is no use for the ventilation. The wind flow volume of the exhaust fan depends on the sizes, short and length and direction of the discharge pipe. It should be 1020m3/min. 2.3.4.4 The ventilation device should be made by metal materials, no plastic materials. dimension of the

- 24 -

Fig.2-2 Installation of Ventilation Device

2.4 Other Requirements


2.4.1. Working bench 2.4.1.1 Dimensions of working bench: 110A/120A/130A: 110B/120B/130B: 300(L) X110 (W) X 70(H) cm 250(L) X 110 (W) X 70(H) cm

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

- 26 -

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.

3.3.1 Necessary Devices


3.3.1.1 Hollow Cathode Lamp (HCL): The user should prepare HCLs to be determined. The HCLs equipped with the instrument are used mainly for adjusting the instrument, surely they can also used for the determination if it it required. 3.3.1.2 Prepare several plastic barrels with volume of 510L for the waste liquid and the deionized water. The barrels for different use must have obvious labels. Glass containers are not used to load the waste liquid. 3.3.1.3 Printing Paper: A4 duplicating paper. 3.3.1.4 Common Tools: Besides screwdrivers and inner hexagon spanners equipped with the instrument, - 27 -

user should prepare some screwdrivers with various sizes, shifting spanners, sharp nose pliers, and so on.

3.3.2 Instrument Installation


3.3.2.1 Take out the main unit, all accessories, parts and components from the packing box. Place the graphite furnace power supply, main unit, computer and printer from left to right sides on the working bench. 3.3.2.2 Put the main unit on the working bench, and ensure that all of its feet are compact with the tabletop. If any not, adjust the four height-adjustable feet and make the instrument balanced and firm.

3.3.3 Connection of main unit with the electric circuit


Wirings of the electronic system inside of the main unit have been well connected before the delivery. Dont change or detach the inter wirings at will unless there are troubles in the instrument, but repair it by the authorized person. The connection of the electric system with the main unit refers to Fig. 3.1. There are three sockets locating at the rear of the instrument, from left to right side: 3.3.3.1 Computer Communication Socket: marked with ion computer with the computer communication cable. 3.3.3.2 Connection Socket with Graphite Furnace Power Supply: Marked with an ion of the graphite furnace power supply, DB-9 male socket. Connect it to the COM socket of the graphite furnace power supply with the cable equipped with the graphite furnace power supply. Pay attention to the label at the cable end. 3.3.3.3 Power Supply Socket: 3-core power socket labeled 198~242V or 230V. Connect it to the city power supply with the cable of the cross sectional area of 1mm2. 3.3.3.4 The power supply cables of computer, monitor and printer are directly connected to the city power socket (the output socket plate of stabilized power supply). , D-9 female socket, connect it to COM2 of

- 28 -

Fig. 3-1 the connections of outer electric systems with the main unit

3.3.4 Installation of flame atomizer (Only for AAS-110B/120B/130B)


Flame atomization system consists of nebulizing burner and gas supply system. Turn the button located on the nebulizing burner to adjust the forth and back, up and down positions of the burner slot to make it aimed at the optical path.

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.

Fig. 3.2 Burner slot adjustment


3.3.4.1 Connections of Gas Pipes for model AAS-110 AAS There is a gas control unit and six jointers located at the rear of the instrument. They are respectively: The inlets and outlets of the acetylene (C2H2), oxygen (O2 ) and air. (1) Gas pipes of the flame atomization system, including the acetylene, oxygen and air, are connected as

- 29 -

the following:
1 C2H2 OUTLET C2H2 INLET;

C2H2 OUT C2H2 INLET of atomizer.


2 AIR OUTLET AIR INLET ;

AIR OUTLET AIR INLET of atomizer;


3 Oxygen sources OUTLET Oxygen INLET;

Oxygen INLET

Oxygen OUTLET of the atomizer.

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.

- 30 -

Fig.3-3 Gas Pipes Connections of Atomization System (AAS-110B Type)

3.3.5 Installation and AAS-110A/120A/130A

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.

- 31 -

UP

FRONT

BACK

DOWN

FLAME

FLAMELESS

Figure 3-4 Integration atomizer control keyboard


Its functions are as follows: FLAME---Press this key to move the flame atomizer into the center of the optical path. FLAMELESSPress this key to move the graphite furnace atomizer to the center of the optical path. UP---Adjust upper position of the atomizer. DOWN- Adjust the position of the atomizer down. FRONT- Adjust the position of the atomizer forward. BACK--- Adjust the position of the atomizer backward. 3.3.5.2 Operation and points for attention After switching on the power supply of the main unit, select the atomizer to be used and press FLAME key or FLAMELESS key, the corresponding atomizer will be automatically moved to the center of the optical path. When the atomizer is reached to the position, press the position keys of UP , DOWN , FRONT and BACK to final adjustment. Selection of the optimal position of the flame atomizer: When entering into the program and completing the initialization, continuously sprays the sample, then observe the absorbance value received as adjust it fine (main adjustment is the vertical direction, or it is adjustment of the flame height), observe the received absorbance until it is up to the maximum. Selection of the optimal position of the flameless atomizer: When entering program and completing initialization, observe the lamp energy, firstly remove the graphite furnace in the horizontal direction (by press FRONT and BACK keys) to search a maximum position of the lamp energy, then remove the - 32 -

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.

3.3.6 Installation of air-compressor


3.3.6.1 If an air compressor with low noise is equipped, please firstly check if 18# freezing oil regulated is injected in the compressor. 3.3..6.2 Be sure that the air compressor itself runs normally before it is connected to the gas control system. Firstly, check if the compressor can start normally after powering on. Secondly, check if the air compressor could satisfy with these requirements: auto-start at a certain pressure (about 0.5MPa) and auto-stop at a certain pressure (about 0.7MPa). Thirdly, check if the oil-water separator and the air filter-reducer run in a normal case, and if the outlet pressure could be adjusted to the expected value (generally 0.4MPa). For an oil free air compressor, do not need to do the above, but be sure that it runs normally before it is connected to the gas control system. 3.3.6.3 The air-compressor is connected to the gas control box according to Fig.3-3 or 3-5.

3.3.7 Installation of gas-water separator


3.3.7.1 Take out the water discharge holder from the accessory box and fix it on the main unit with screw the three screws equipped as shown in Fig. 3-6.

- 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. Installation of Oxygen Source


3.3.9.1 Oxygen source is generally stored by a steel cylinder equipped with pressure regulator. The outlet pressure of the regulator is in the range of 0~0.25MPa. If the general pressure inside of the cylinder is less than 0.5Mpa, new one should be replaced. Keep the inner of the oxygen pipes cleaning to avoid blocking the gas piping components and parts.

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.

3.3.10. Connections of Waste Liquid Piping (Shown as in fig.3-7, 3-8)


3.3.10.1 For Model AAS-110B/120B/130B, there is a waste liquid nozzle on the atomization system (at the front bottom of the atomization chamber). Use 1.5m long, 8 (internal diameter)1.5mm plastic pipe to connect its one end to the waste liquid nozzle as the waste liquid discharge piping. Make a 15cm circle in the middle of the plastic pipe, and it is fixed. Add a small amount of water into the plastic pipe and remain it at the water seal and keep the water seal level above a half of the circle height, shown as in fig.3-7, to make the inside of the atomizer kept away from the outer atmosphere. Insert the other end of the waste liquid pipe to a 5-10L plastic bucket. But never insert it into the waste liquid bucket. Dont insert the waste liquid tube directly to the waste water system of the Laboratory so as to avoid corrosion piping. 3.3.10.2 For Models AAS-110A/120A/130A, there is a waste liquid nozzle on the atomization system (at the front bottom of the atomization chamber). Use 0.5m long, 8 (internal diameter)1.5mm plastic pipe to connect its one end to the waste liquid nozzle as the waste liquid discharge piping. The other end is connected to the top end of the jointer of the water seal fixed at the edge of the working bench, fill in water with the water seal to keep its height of the water level as shown in Fig. 3-8, in order to make the inside of the atomizer kept away from the outer atmosphere. Again connect a plastic tube with the same size at the jointer of the button end of the water seal and insert it into 5-10L plastic bucket. But never insert it into the waste liquid bucket. Dont insert the waste liquid tube directly to the waste water system of the Laboratory so as to avoid corrosion piping. NOTE: To avoid flashback, explosion or gas leakage, be sure that the water seal must be in good

- 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.

Fig. 3-7 Connections of Waste Liquid Pipes for AAS-110B/120B/130B

Fig. 3-8 Connections of Waste Liquid Pipes for AAS-110A/120A/130A

3.3.12 Installation of Hydride Atomization System


AAS series models all can select the hydride-generator and the quartz- tube furnace for the hydride method. About the operation guide and installation method of this accessory, please refer to its own instructions.

3.4 Acceptance Inspection


After the installation of the instrument according to the above requirements and rules, the acceptance inspection can be made afterwards. Before the acceptance, firstly, read the operation manual carefully and master the functions of all buttons and knobs until the operation procedures are all known well. And power on the instrument. Unqualified operators can never be allowed to operate the instrument. DO NOT change the instrument software and parameter files randomly; otherwise the operating troubles may be occurred. The purpose of the acceptance inspection is to check if the quality of the instrument has some change after the transportation or the storage for a long time. If it is so, please find the reasons to repair it well. - 38 -

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 -

Chapter 4 Software Operation


This software runs on Windows98 XP operation system. Master the operation of Windows98 XP before using this software.

4.1 Enter the Software


Power the instrument and the computer on. The computer automatically enters Windows 98 desk or XP operation system desk, starts successfully, double click the shortcut icon with the name of AAS Analyst on the desktop, and then you enter the software as shown in Fig.4-1.

Fig.4-1

4.2 Edit Analytical Method


Select Operation>>Edit Analytical Method (M) from the menu and youll see the Operation Dialog as 1 Analytical Light Source: The flame atomic absorption analysis, the graphite furnace shown in Fig.4-2. atomic absorption analysis, the hydride atomic absorption analysis and the flame atomic emission analysis 2 Operation: It can be used to create a new method, modify the existed all can be made by this instrument;. method and delete the existed analytical method. User could directly click the analytical method as shown in Fig.4-2 according to the analytical requirement. For example, user wants to select the flame atomic absorption method. Click Flame AAS and Create, so they are selected. And then click Continue, the Creation of method dialog will pop up, as shown in Fig.4-3. To select analytical element, click button as shown in Fig.4-3 to appear the Element period table as shown in Fig.4-4. Click certain of - 43 -

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 -

4.3 Setting of Analytical Conditions 4.3.1 Selection of Instrument Condition


1 Wavelength: Refer to Fig.4-5, click Instrument condition label to select the instrument condition.

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

4.3.2 Selection of Measurement Condition


Click the Measurement Condition tab in Fig.4-5, and appear Fig.4-6.
1 Analytical signal: Including Time average (flame method), Peak height and Peak area (graphite

furnace method or hydride method).


2 Measurement mode: Including STD calibration (standard working curve) and standard addition

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

4.3.3 Setup Standard Working Curve


Click the Working curve tab in Fig.4-5, and appear Fig 4-7.
1 Equation: A linear equation or a quadratic equation is selectable.

- 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

4.3.4 Setting of Flame Condition

- 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.

4.3.5 Quality Control (Re-slope)


Click the QC tab in Fig.4-5 to appear the page as shown in Fig4-9.
1 Auto-re-slope: If the auto-re-slope is selected, please click Auto-re-slope located in front of the

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 -

4.4 Selection of Graphite Furnace Conditions (Only for AAS110A/120A/130A)

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,

the main gas is closed.


2 Record: This column means that the base line zero signal and collecting sample signal are sent to the

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.

4.5 Selection of Hydride Generator Method Condition


Refer to Fig.4-2, click Hydric Generation AAS and Create, and then click Continue. The following procedures refer to the section 4.2 and 4.3. The difference is in Fig.4-5, the Condition of hydric generator will be instead of the Flame condition as shown in Fig.4-11.
1 Deoxidizer: Click Deoxidizer to select NaBH4 or KBH4. 2 Carry-gas flow, Heating, Observing height: Input these parameters according to the analytical

conditions of the element to be analyzed. The analyzing operations are the same as the flame AA method.

- 52 -

Fig. 4-11

4.6 Flame Atomic Emission Method (only for AAS-110A/110B/120A/120B)


The operation procedures of the flame atomic emission are the same as that of the flame atomic absorption method. Refer to the section of 4.2 and 4.3.

4.7 Modify Existed Method


If the inputted conditions are required to be modified, please follow the following operation procedures: Click Operation>>Edit Analytical Method in Fig.4-1. Then select Modify in Fig 4-2, afterwards, Continue to appear Fig.4-12. If any of method is required to be modified, double click to change it into blue color, then click OK to return to Fig.4-5. Refer to the section of 4.3 to modify it such as: Instrument condition, Measurement condition etc.

- 53 -

Fig. 4-12

Fig. 4-13

Fig. 4-14

4.8 Delete Existed Method


If any of the existed method is required to be deleted, please follow the following procedures: Click Operation>>Edit Analytical Method in Fig.4-1. Click Delete and Continue in Fig.4-2 to appear

- 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.

4.9 Selection of Analytical Method


When the creation method is set well and no change at all, as shown in Fig. 4-2, click Finish in Fig.4-2 to go back to Fig.4-1. Click File>>New from the menu to appear the dialog frame as shown in Fig. 4-13. In Analytical source, click the Flame AAS and OK to appear the page as shown in Fig.4-14.

4.10 Analytical Project Design 4.10.1 Method Selection


In Fig.4-14, click the first column of Element line and Lamp# line and make them blue. Then click Method to appear the page as shown in Fig.4-12. Click the element to be analyzed and click OK. The page is returned to Fig. 4-14, the moment, the first column has been selected in Fig.4-14. If more elements are required to be selected, repeat the above steps and up to six elements can be analyzed in one project.

4.10.2 Sample Table

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.

4.10.3 Save Sample Table


If user wants to save the sample table in the section 4.10.2, click Save sample table in Fig.4-14. Input the file name to be saved and click Save. This file can be used for the future analysis.

4.10.4 Load Sample Table


Click Load sample table in Fig.4-14 to select the existed file name, click Open, then the sample table is loaded. It can be modified again.

4.10.5 Delete Items


Refer to Fig.4-14, If the modification or the deleting is required, click the method selected to be blue, which is beside Element and Lamp position, again click Delete a project to delete it immediately. To select a new method, click Method and select a new one again. When the analytical project design is finished, click OK to appear the page as shown in Fig.4-16.

- 56 -

Figure 4-16 4.10.6 Instrument Control


1 Main light beam: It is selected by the routine method. It is used to adjust the negative high voltage

(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

and Reference up to the balance.


5 Auto-wavelength: Click Auto-wavelength to appear the page as shown in Fig.4-17. The moment, the

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 -

make auto-balance (Only for models AAS-130A/130B).


7 Wavelength scan: It shows the energy distribution of the scanning spectral line in the designated

wavelength range as shown in Fig.4-18.

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

background value during printing in details.


3 Show temperature: If select ,that means that the temperature curve will be displayed during the

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

4.11.4 Standard Addition Method


When the co-existed substances are not so clear in the sample or the content of the matrix is very high and variable, the standard solutions is hard to be prepared. In such a case, it had better using the standard addition method. Divide the sample into four equal parts, and respectively add unequal standard solution into the second, third and fourth parts. Then dilute the four samples to be equal volume for the determination. - 68 -

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 -

4.12 Flow Diagram

- 70 -

Chapter 5 Enriched Oxygen Air-Acetylene Flame


5.1 Introduction of enriched oxygen air-acetylene flame
Enriched oxygen air-acetylene flame atomic absorption spectral method is a new type of high temperature flame AAS method. Its advantages are: environmental protection, cost, easy-used and large available range. Generally, the flame AAS includes two types. One is air-acetylene flame AAS. This flame temperature is 2300 OC, so it is only used for the first class elements, whose melting point and boiling point are all lower (<2000OC) and oxide dissociation energy is less than 5eV, such as alkali metals, Cu subunit, Zn subunit, Mn, Te, Co, Ni, Pb and so on. For the second-class elements, whose the melting point and the boiling point in the middle and oxide dissociation energy is about 5eV, such as alkaline-earth metals, Cr, Mo, Ga, Ge, Se and so on, the atomization efficiency is lower and the serious solute interference (chemical interference) will be occurred when using this flame method, because the flame temperature is comparatively low. For the third-class elements, whose high melting point and high boiling point and oxide dissociation energy is more than 6eV, such as rare earth elements, Ti subunit, V subunit, W, P, Al, Si and so on, this flame can not be used any more. The other is N2O-acetylene flame AAS. This flame temperature is up to about 2950OC.It is high temperature flame. Its temperature is 650 higher than the temperature of the air-acetylene flame. For the second-class elements, the atomization efficiency is improved remarkably and the chemical interference is overcome using this flame. This flame can be also used for the third-class elements with high melting point and high boiling point and high oxide dissociations energy, In this case, up to about 70 elements can be determined. However, this flame has some defects. Such as: much of poisonous gas (laughing gas) is used, the cyanogens molecule (CN) will be generated when burning. The consumption of N2O is large and expensive. And the temperature of this flame is hard to be adjusted, so it is hard to obtain the optimal atomization efficiency for the second-class elements, and has strong CN molecule emission or absorption, which will affect the sensitivity of some elements. The temperature of the air-acetylene flame is comparatively low because the oxygen content in air is low while N2O can produce higher ratio oxygen during the high temperature dissociation and it releases much heat energy, which makes the flame being up to 2950 OC. In 1965, Mr. Amos ever tried to test the oxygen-acetylene flame and N2-oxygen-acetylene flame, which the - 71 -

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 Operation of enriched oxygen air-acetylene flame


The operations of the enriched oxygen air-acetylene flame are the same as that of the air-acetylene flame AAS. The main thing is to master how to adjust the mixing ratio of the acetylene and the oxygen. Note 1) Firstly increase the acetylene flow and then increase the flow of the oxygen; .2) General pressure of the acetylene cylinder is more than 0.6Mpa. Do as the following: - 72 -

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 -

- 74 -

Chapter 6 Maintenance and Service


This chapter is compiled to help user master the fundamental of AAS and solve the problems during the determination.

6.1 Attention Points for Maintenance


When troubles occur during running the instrument, please diagnose the abnormal phenomena and process them according to this chapter. If the user could not solve the problems, please contact to your local authorized distributor to solve it. In addition, Read the operation manual carefully before running the instrument due to the user being unfamiliar with the operation of the instrument. This chapter gives you the attention to the maintenance, however, some base but important things should be emphasized here before the user makes the maintenance on the instrument. Caution: Some parts of instrument can not be re-mounted after detaching it. So do not dismantle any part of the instrument at any time unless you have got the authorization to do so. The following should also be noticed when making the maintenance: 6.1.1. Do disconnect the power cables before dismantling the instrument. 6.1.2. Cut off the water source and gas sources before the maintenance. Close the total valves of all gases, especially the acetylene cylinder. 6.1.3. Do not leave bolts or screws, and so on inside of the instrument. If so, must take them out. 6.1.4. Do not touch the surface of optical parts when maintaining inside of the monochromator. Never set the high voltage (gain value) of PMT when the monochromator is opened. 6.1.5. Do not damage the printed circuit board when making the maintenance.

6.2 Replacements and Adjustments of Components and Parts


Some parts of AAS are consumables or vulnerable parts, so they need to be replaced after a period of time use. For example, D2 lamp, HCL, graphite tube, and graphite cone are consumable parts, and nebulizer, bump ball and burner are vulnerable parts. Those parts are easily corrosive. The replacement is required. Some of the other parts are not consumables or vulnerable parts, but they will be rusted after working for a long time, such as optical parts, electric parts, etc. Anyhow, the damaged parts must be replaced. For securing the good performance of the instrument, some parts should be adjusted after the replacement.

6.2.1 Replacement and Adjustment of HCL (Hollow cathode lamp)


Hollow cathode lamp is the main light source of the instrument and its life is generally 5000 mA/hour. The - 75 -

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.

6.2.2 Replacement and Adjustment of D2 Lamp


1) The minimum lifetime of D2 lamp is 500 hours. It should be replaced when its lifetime is over. During the replacement, the outer dimension must be the same as the original one, and its working parameters should meet the requirements of the instrument: Anode Current: 300mA

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!

6.2.3 Replacement of Nebulizer


Nebulizer is the key part of the atomization system. Analytical sensitivity and detection limit greatly depend on the working status of the nebulizer. This part is unique channel for the sample entering the atomization system, so pipetting capillary, nozzle and impact bead will be directly corroded by the sample solutions. Wash these parts with de-ionized water after every analysis. If the instrument works badly, check if the nebulizer should be replaced and washed. Replacement method: 1) Unscrew the four screws on the front of the nebulizer and take off the small bended angle. 2) Take off the impact bead from the nebulizer slightly. 3) Pinch the metal holder on the back of the nebulizer and take it off slowly. If it needs to be washed, dip its glass part in acid solution. 4) Install the washed nebulizer or a new one slightly according to the above 3~1 steps. Note: (1) When installing the nebulizing nozzle, leave its neck down. Otherwise, the stability of the instrument will be affected. (2) When screwing the four screw of atomization chamber, do not forget the O-rings on the front cover. The four screws should be screwed equably tightening, avoiding the flashback.

6.3 Daily Maintenance 6.3.1 Light Source


1) Hollow Cathode Lamp (1) Carefully install or detach HCL to avoid breaking. Keep the light passing window clean. If oil stain or fingerprint dirties the window, the light energy emitted from the cathode will be decreased, especially for the energy of the short wave. To clean the oil stain, wipe the window with absorbent cotton dipped with alcohol-ether mixture solution (ratio 1:3). Hold the lamp holder when taking the lamp up or down. (2) HCL cannot be placed without using for a long time. Otherwise, it will not be ignited or used normally because of gas leakage, gas absorption or release. Power on those rarely used HCLs for 2~3 hours every 3~4 months. It is very important for avoiding the batch obsolescence. - 77 -

(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.

6.3.2 Optical System


1) Keep the lens in the lamp chamber, the lens exposed in atomization chamber and the top of photosensitive probe clean, and dont touch them with the fingers. 2) The beam joiner in the lamp chamber is constructed by aluminized half-reflection lens. The lens must not be touched with the fingers or wiped with anything. 3) The dust on the lens can be removed by rubber blowing ball or be slightly wiped by the cleaning lens paper. 4) If the oil stain or the fingerprint dirties the lens, wipe them slightly with absorbent cotton dipped with alcohol-ether mixture solution, but be careful not to leave scratches. 5) Do not open the monochromator closure in a hurry. If it has to do so, firstly set the PMT high voltage as 0V. Do not touch the surfaces of the grating and the spherical reflectors, and never wipe them with lens paper or absorbent cotton. 6) Do not talk, breathe out or spatter saliva directly facing to the grating. Dust on the grating can be removed by cleaning rubber blowing ball.

6.3.3 Atomization System


Samples of AAS are generally corrosive. For securing a long time use and high performance of the instrument, the atomizers should be maintained regularly, including the flame atomization system and the graphite furnace atomization system. 6.3.3.1 Nebulizing Burner System 1) Daily Cleanness and Maintenance 1 Keep the flame on and spray the de-ionized (1) Do the following after a batch of samples are analyzed: 2 Clean the water for about 10 minutes. Thus it can remove the left samples in the analyzing system. 3 Pour out the waste liquid in time. overflow sample drops, especially organic drops. (2) Routine Maintenance. Clean the nebulizing burner system weekly, including the nebulizer, the

- 78 -

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.

6.3.4 Gas Supply System


The gas supply system of the flame method includes gas control unit, air compressor, oxygen cylinder, acetylene cylinder and gas pipes. The gas supply system of the graphite furnace method includes gas control unit, argon cylinder and gas pipes. The maintenances of the gas supply system are as the following: 1) Check the pipes, valves and connectors for the gas leakage regularly. If there is the gas leakage, repair or replace it immediately. 2) Often check if there is water in the loop of the air compressor. If so, drain it off in time. Often drain off the water in the gas-water separator to avoid the water entering into the gas flow meter. For the oil air compressors, drain off the water and oil in the filter and the storage tank regularly and often check if the oil is required to be filled with.

6.3.5 Circuit System


1) If the instrument has not been used for a certain time, it should be powered on regularly to avoid the damage to the circuits, especially in the moist area. For avoiding short circuit caused by wetting and mildew and avoiding the corrosion of electric parts, the instrument should be covered by a dust proof cover. 2) For the instrument often-used, the dust on the circuits should be cleaned regularly. Cleaning method is: pull the circuits off and blow them with rubber ball or remove the dust with soft hairbrush. After cleaning, install them as the original appearance. Ensure that plug those cables and connectors rightly.

6.4 Circuit Schematic and Function Description 6.4.1 General Description


Models AAS-110A/110B/120A/120B/130A/130B instruments circuits mainly include two parts: a right electric box is a main board and the left electric box is the gas control unit. Model AAS-130A/130B are provided with four lamps. The electric diagram is shown in the following figure.

- 80 -

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.

- 81 -

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.

6.4.3 Gas Control Board (PC5)


See the schematic diagram of gas control board as following:

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.

- 83 -

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.

6.4.4 Signal Amplifier Board (PC2)

Signal Amplifier Board - 84 -

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.

6.4.5 Control Board (PC3)


Programmed chips are mounted on this board. Do not dismount or replace this board in a hurry.

6.4.6 Motor Control Board (PC4, PC6, PC8, PC9)


The fundaments of these boards are all the same, optical coupler is used as the position feedback. Power supply is +5V. When both ends of the LED in the optical coupler is applied on about 2.5V voltage, the CE end will vary if something shield the light emitted by the LED (vary from 0 to 5V). The CE signal will control the rotation of the motor.

6.4.7 Integration Atomization Control Board (PC12)


As shown in the following figure:

Schematic diagram of integration atomization control board


1) Socket: Interface of keyboard. 12TP1 is GND; 12TP2 is +25V; 12TP3 is +5V. 2) Socket: Limit protection. 3) Horizontal optical coupled socket: Pin 1 to GND; Pin 3 is low level when light is passing through the optical coupler. When the light is blocked, it shows high level. 4) Vertical optical coupled socket. Pin 1 to GND; Pin 3 is low level when light is passing through the optical coupler. When the light is blocked, it shows high level. - 85 -

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.

6.5 Trouble Shooting 6.5.1 Treatment with Emergency


(1) Suddenly Power Off In this instance, switch off the instrument, computer and other devices rapidly, and cut off all the gas sources. When everything is OK, again power on the instrument according to the operation procedures. (2) Flame Color Abnormal and big change This means the combustion gas is seriously polluted. The normal color of the air- acetylene flame is baby blue. In this instance, cut off the acetylene source immediately. Purify the acetylene gas and ignite it again.

6.5.2 Changes of Wavelength Parameter


Because of the transportation, shock or other reasons, the wavelength translation or nonlinear movement will be occurred. On this occasion, the instrument parameters should be reset. 6.5.2.1 Adjustment of Wavelength Translation. The wavelength value displayed on the computer has the deviation of the equal value with the system real wavelength value in the same direction of the whole wave section, so it is called as Wavelength translation. The adjustment methods are: 1) Power on Cu lamp and set the lamp current to be 3mA. Put Cu lamp into the optical path, then click Wavelength scan key in Fig.4-16 to appear Parameters of Scanning as shown in Fig.4-18. 2) In Start Wavelength and End Wavelength frame, respectively input the wavelength value of the start end (320.0nm) and the wavelength value of the ended wavelength (330.0nm). Input the working voltage of PMT (230~260V) in gain frame. Click OK key to start the system scanning (there is running sound in the monochromator) and appear the page of the wavelength scanning. 3) If the wavelength range and the working voltage are properly selected, when the scanning is completed, the graphics will be appeared in the black frame of the page as shown in Fig. 6-1. That is: 324.7nm and 327.4nm of Cu and a small peak nearby. Use the mouse respectively to aim at the top end of the peak shape, the real wavelength value X is displayed on the page, respectively obtain X1 and X2.

- 86 -

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.

- 87 -

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).

- 88 -

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.

6.5.3.2 Troubles of hollow cathode lamp


Phenomena No light. Reasons Lamp power supply is damaged or not connected well or Fuse is damaged. Solution Check if the voltage of 1TP11 on main board is normal. Check the connections of all sockets. Lamp has gas leakage. Only emit light from the outside of cathode; low measuring line energy; high working voltage. Glowing color is normal, but energy of analyzing line is too low, even hardly to be detected. For long time use, the cathode metal is exhausted or the radiation intensity of weak light elements (As, Te, Se, Bi, Sb, etc) is too low. The lifetime of lamp which cathode metal is exhausted is ended. Replace a new lamp. Select the lamp with big intensity instead of weak light elements. Sensitivity is lower during determination. Emitting background of lamp is too big. Replace a lamp with low emitting background if the low sensitivity is caused by the lamp. Light from the lamp is very strong and lamp current is Lamp circuits have problems. If only one lamp has this problem, it shows its power Pressure intensity of inert gas is decreased too low to support the normal discharge.. Replace a new lamp. Lamps lifetime is over. Replace a new one.

- 89 -

also very large.

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.

Replace a new lamp.

6.5.3.3 Light source is normal, but no energy is displayed after scanning.


(1) Touch the Pin2 of the pre-amplifier on the amplifier board slightly with fingers and observe if energy is displayed. 1 There is no output voltage on the (2) If the energy is displayed, the three reasons may be the following: HV module. Checking method: In the page of Instrument Alignment, set the voltage of 300V and measure the shielded wire of HV module if there is 300VDC voltage output with the universal meter in the range of 500~1000VDC. If it is not, measure the control plug of HV module. Red wire should be +15VDC and white wire should be +1.5VDC. If these two voltages are normal, that shows the HV module is damaged or the plug is not connected well. If these two voltages are abnormal, that shows the problems may occur on the main board. Please switch off the instrument and check if all the chips and plugs are connected well. If the problems cant be still solved, contact with the local distributor or the manufacture. 2 Wavelength Translation. See the section 6.6.2. 3 Wavelength Nonlinearity. See the section 6.2.2. (3) If no energy is displayed, check if the 15V, +5V on the main board are normal. If it shows abnormal case, it may be caused by poor contact of ~18V plug and ~8V plug. Check all the lines of these two plugs after switching off the instrument. If the voltage is normal, please switch off the instrument and check if all the chips and plugs are connected well. If it still cant be solved, contact with the local distributor or the manufacture.

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.

6.5.3.6 Auto-wavelength (or setting of wavelength) is abnormal


(1) When running auto-wavelength (or setting of wavelength), the scan motor can not be stopped for a long time, the moment, switch off the instrument immediately. If there is no any action after re-testing, set the HV (gain) to be 0V and open the monochromator to check the optical coupler of the wavelength controlled motor blocks the light well or damaged, referring to the section 6.4.6. (2) Abnormal sounds occur during the self-check of the slit mechanism and the lamp turret, check their optical couplers.

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.

6.5.3.8 Instrument Alarm


Phenomena Start alarm and alarm lamp is on when powering on the instrument. Reason Gas sensor alarm. Instrument parameter Is changed caused by the environmental changes of the instrument. Solution Adjust 5RP3 according to the section 6.5.3.

- 91 -

Alarm when Igniting failure.

There is air in the acetylene pipes.

Re-ignite for more times and remove the air out from the pipes.

Instrument parameters are changed.

Adjust 5RP1 or 5RP2 according to the section 6.5.3.

Acetylene flow is too low. Air pressure is not big enough.

Adjust it to about 2L/min. Adjust outlet pressure to 0.2MPa more.

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.

Light sensor alarm.

Adjust 5RP2 referring to the section 6.5.3.

Air pressure sensor alarm.

Adjust 5RP1 referring 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.

Emission of hollow cathode is weak. Optical system is not adjusted well.

Lens is polluted seriously.

Clean the lens with alcohol-ether mixture (ratio 1:3) or replace it.

Slit or optical parts are dirty.

Clean the optical parts or replace them. See the section 6.4.2.

Performance of HV module is decreased.

Replace a new one.

6.5.3.10 Instrument is unstable when the flame is on and spraying.


- 92 -

(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

- 93 -

(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

- 94 -

Troubles in electric system.

Some components are damaged in the circuit. Hard magnetic field or high frequency interference.

Repaired by manufacture.

Far away from the interference sources.

6.5.3.11 Results have the problems. (1) Sensitivity is low.


Reason Wavelength is not correct. Flame property is not right. Flame position is not right. Solution Sole it according to the section 6.6.2. Refer to the concerned manuals. Adjust the burner up or down, front or back and its turning angle. Nebulizer is not good enough and spray efficiency is too low. Lamp current is too large. Adjust the position of impact bead or replace a new one. Decrease the lamp current to improve the sensitivity but will affect the stability. Slit is too wide. Choose the proper slit according to analysis manuals. Nozzle is blocked up and sampling flow volume is too low. Atomization efficiency is low because of sample concentration, vapor tension or matrix concentration. Properly process the samples and change their physical properties. Clean the nozzle or replace a new one.

(2) Detection limit is unqualified.


Reason Integral time is not long enough. Sensitivity is too low. Noise is big. Spray is unstable. Solution Increase the integral time. Solve it referring to the above table. Increase the lamp current properly Check the nebulizer.

(3) Results are comparatively low.

- 95 -

Reasons Matrix or chemical interference exists.

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.

(4) Results are comparatively high.


Reasons Reagent blank has not been used for the calibration. Ionization interference exists. Standard solution is prepared inaccurately or is metamorphic and its real concentration is lower that the calculated value. Method is not properly.. Change other wavelength, use background corrector or higher temperature flame. Re-prepare standard solution, adding de-ion agent or ionization proof agent. Solution Use the reagent blank to calibrate it again.

(5) Calibration curve doesnt pass through zero point.


Reason When preparing the samples, the agent or solvent used is polluted. Solution Re-prepare the sample solutions.

(6) Results drift


Reasons Lamp is not pre-heated enough and is still unstable. Intensity is always changed. Frequently adjust lamp current. Replace a stable lamp or auto-adjust the zero. Pre-heat ten minutes after changing the lamp current. Solution Prolong the pre-heating time.

- 96 -

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.

Solution temperature is changed.

Check and eliminate it.

6.5.3.12 Flashback occurs


Reasons No water seal at draining outlet of waste liquid . Burner slit is widen. Oxygen content in air steel bottle is too large. Acetylene flow is too low and oxygen flow is too high when using the enriched-oxygen airacetylene flame. Replace the burner. (Slit width < 0.7mm) Replace the air steel bottle. After ignition, firstly increase the acetylene flow, and then increase the oxygen flow. Repeat these two steps. Add a water seal. Solution

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.

6.5.3.13 Abnormal running of graphite furnace method


Reasons the graphite furnace power supply system cant be powered on Solution Communication cable is not connected. After changing the parameters of graphite furnace power supply, firstly click Read key in the dialog. Power supply of graphite furnace runs abnormally. Energy is low. See the operation manual of graphite furnace power supply system. Adjust the up and down, forth and back positions of graphite furnace.

6.5.3.14 Troubles of background corrector (1) D2 lamp is not lit


- 97 -

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.

Setting of the software is not correct.

Set reference signal to be D2.

(2) D2 lamp energy is low.


Reasons Light spot of D2 lamp has not been entered into the optical path. Wavelength range used is not correct. The short wave range should be used for D2 lamp (<300nm). D2 lamp lifetime is over after long time use. Replace a new one. Solution Re-adjust the position of D2 lamp.

(3) Noise is large when using background correction.


Reasons Energy of D2 lamp is low, so that HV(Gain) is too high. Solution Adjust the energy of D2 lamp and decrease the high voltage. If the energy can not be adjusted any more, the slit will be widen. Damps of both background correction circuits are small. Not faulty.

(4) Background correction effect is not good enough.


Reasons Electric balance is bad. Optical balance is bad. Solution Customer cannot adjust it. Re-adjust the positions of D2 lamp and HCL and make the two light spots overlapped. Concentricity of light spot of HCL is bad. Rotate hollow cathode lamp to seek the overlapping position of both light spots.

- 98 -

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.

6.5.4 Usage and Maintenance of Computer


6.5.4.1 Attentions to using computer. (1) Do not disconnect the communication cable when the instrument or the computer is powered on. (2) Avoid frequently power on /off the instrument or the computer. (3) When switching off the computer, do the following steps: click Begin>> Close System>> Close the computer>>Yes. Dont press its switch directly. (4) Computer should be far away from strong magnetic field. (5) Do not plug or insert floppy disk when the indicator is on. (6) Update the old parameters or change the instrument parameters only by the specialized engineer. (7) Save modified parameters in time to avoid loosing data. (8) During operating the computer, if the mis-operation occurs, the computer will be dead. 6.5.4.2 Software backup and installation. (1) Software backup: Backup the software if user wants to update the operation system or change a computer. (2) Software installation: For example as the installation of Model AAS-110 software Insert the setup floppy disk or CD equipped in the accessory box into the light driver and open it; Double click AAS 110 setup.exe; Appear window :This will install AAS110. Do you wish to continue, click Y; Appear window: setup-AAS110 click Next>; Appear the following window, click Next>.

- 99 -

Appear the following window, click Next>.

Appear the following window, click Next>.

- 100 -

Appear the following window, click Install.

After the computer is automatically installed, appear the following window, click Finish.

- 101 -

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.

- 103 -

S-ar putea să vă placă și