Flame Spectrophotometer FP64350 Operating Procedures

Flame Spectrophotometer

Flame Photometer is an analytical instrument based on the basic principle of emission spectra. Includes: Gas and flame combustion part, optical part, photoelectric converter and inspection record part. The process is to spray the specimen into the flame by a nebulizer, excite the light, after splitting the light by the detector to measure the emission intensity, the latter is proportional to the content of the element to be measured in the specimen. such as: When the salt is placed in the Flame photometer, the flame is yellow, which is due to the sodium atom in the salt of the outer layer of the electron to absorb the heat of the flame, and jump to the stimulated energy level, again by the excited energy level back to normal state, the electrons will release energy. The characterization of this energy emits a spectral spectrum of spectral bands with wavelengths peculiar to the sodium atom. By using the heat of the flame, the atoms of an element are excited to emit light, and the strength of the spectral energy is detected by the instrument, and the content of an element in the substance is judged, and this kind of instrument is called the Flame photometer. Today's more advanced flame photometer can simultaneously carry out multi-element simultaneous analysis and detection, integrated air compressor design, and with Software records.

The flame photometric method is quantitatively analyzed by Romadin formula, i.e.I=AXCof thebThe second party, in the formulaIfor the intensity of the spectral line,Cis the content of the element to be measured,Dis a constant related to the evaporation and excitation conditions of the element to be measured;bfor the self-absorption coefficient, because the flame as the excitation light source, its temperature can be controlled by air and gas flow to maintain stability, but also because of the use of liquid samples, the composition of the sample has less impact, so in each testais a stable constant, generally due to low sample concentration, self-priming negligible, soI=λc, and can be analyzed by means of relative strength measurement.

For flame photometric analysis, the liquid to be measured with a nebulizer into the Sol into the flame, the element to be measured due to the thermal dissociation generated ground state atoms, in the flame is excited to produce a spectrum, after the monochromator decomposition into a single shade by photoelectric system measurement, because the flame humidity is relatively low, it can only excite a few elements, Moreover, the spectra are relatively simple, the interference is small, and the flame photometric method is particularly suitable for the determination of alkali metal and alkaline earth metals which are more easily excited.

In order to stabilize the flame and eliminate the interference of some elements, it is often added in the measurement solution."buffering Agent", such asK, Ca, Mgat the same time there is an impact on the determination of each other, if the three elements of the saturated solution as a"buffering Agent", when added to a certain amount in the test solution, the effect is a single constant value, can be used as a background deduction, sodium measurement, a large number ofhco32-the presence of the results can be low, can be used hydrochloric acid test solution after heating removal.


Application examples


1)detection of Sodium:

1a)detection of sodium content in raw pine oil;1b)to detect the exchangeable sodium content in soil;1c)Detection of fuel(crude oil, petrol, diesel)in the sodium content;1d)detection of sodium content in glass samples;1e)to detect the sodium content in straw and forage;

2)detection of sodium and potassium:

2a)Detection of silicate, Inorganic Ore,the content of sodium and potassium in metal ores;2b)detection of sodium and potassium content in fruit juices;

3)detection of Potassium:

3a)detection of potassium content in fertilizers;3b)detection of potassium content in plant samples;3c)to detect the available potassium content in soil;3d)detecting the potassium content in the resin mixture;3e)detection of potassium content in glass samples;

4)detection of Lithium:

4a)detecting the content of lithium in lubricating oil and grease;

5)detection of calcium:

5a)detection of calcium content in beer;5b)detection of calcium content in biological liquids;5c)assess the calcium content in milk;5d)The simplest flame photometric measurement of calcium content;5e)detection of calcium content in fruit juices;5f)detection of calcium content in biscuits and hard bread;

6)Barium Detection:

6a)The simplest flame photometric measurement of barium content;

7)detection of base metals:

7a)detection of alkali-based metal content in cement

8)Sulfate detection:

8a)The simplest flame photometric measurement of sulfate;


4.Impact Factors


Lamp current
The Flame atomic absorption spectrophotometer uses the light source mostly hollow cathode lamp, the hollow cathode lamp operation parameter only one lamp current. The lamp current size determines the radiation intensity of the lamp. Increasing the lamp current in a certain range can increase the radiation intensity, while the lamp stability and signal-to-noise ratio also increase, but the instrument sensitivity is reduced. If the lamp current is too large, it will lead to self-erosion of the lamp itself and shorten the lamp service life.;discharge is not normal, so that the lamp radiation intensity is not stable. Conversely, in a certain range to reduce the lamp current can reduce the radiation intensity, the instrument sensitivity increased, but lamp stability and signal to noise ratio decreased. If the lamp current is too low, it will reduce the intensity of the lamp radiation, resulting in a serious loss of stability and signal-to-noise ratio can not be used. Therefore, in the specific detection work, such as the concentration of the sample is high, the use of larger lamp current to obtain better stability;If the measured sample concentration is low, then in order to ensure the stability to meet the requirements of the premise, the use of low lamp current to obtain better sensitivity.




Atomizer
The Nebulizer function is to spray the test fluid. It is an important component of atomic absorption spectrophotometer, and its performance has a significant effect on the determination of sensitivity, precision and chemical interference. The more stable atomizer spray, the smaller the droplet uniformity, the higher the atomization efficiency, the higher the sensitivity, the better the precision, the smaller the chemical interference. The Nebulizer regulation is now achieved by manually adjusting the relative position between the impact ball and the capillary. The tester should adjust the atomizer to droplet small and uniform, preferably droplets in the surrounding sphere evenly distributed, if not realized, the droplet to the impact of the ball as the center symmetrical distribution can also.




Lifting capacity
The size of the lift affects the sensitivity level. High or low lift will cause nebulizer atomization instability. Each manufacturer's instrument lift range varies, each has a certain range of changes. The measures to increase the amount of ascension are:(1)increase the flow of gas to help. This increases the amount of lift by increasing the negative pressure. (2)shorten the injection tube length. Shortening the tube length makes the pipe resistance decrease, and the flow rate of the test fluid increases. Conversely, if you want to reduce the amount of lift, you can reduce the gas flow or increase the length of the sample tube.




Analysis Line
Each element has many lines of analysis, usually with the highest sensitivity of the resonant line, often used as an analytical line, but when measuring a higher concentration sample, the sensitive line is chosen. For example, for sodium measurementa=589.0nmused as analysis line at higher concentrations330.0nmas an analysis line.




Burner position
Adjusting the burner height and the position of the front and rear, so that from the hollow cathode light beam through the free electron concentration of the largest flame zone, this time the highest sensitivity, stability best. If high sensitivity is not required, the sensitivity can be reduced by rotating the burner angle in order to facilitate the detection of high concentration test fluid.




Flame
The flame type and state play an important role in sensitivity, and the different flame should be selected according to the characteristic of the element under test. Currently the flame is divided into air by type--hydrogen Flame, air--acetylene flame, nitric oxide--acetylene flame. Air--the flame temperature of the hydrogen flame is lower, which is used to determine the elements such as arsenic and selenium that are easily atomized in the flame. Air--acetylene flame belongs to the medium temperature flame, which is used to determine the more difficult elements such as magnesium, calcium, copper, zinc, lead and manganese in the flame. Nitric oxide--acetylene flame is a high temperature flame, which is used to determine the elements such as vanadium and aluminum that are difficult to dissociate in flame. Flame according to the state of the poor flame, chemical measurement flame, Fu. Poor flame refers to the use of excessive oxidants when the flame, because a large number of cold oxidizing agents to take away the heat of the flame, this flame temperature is low, and due to the full oxidizer, burning completely, the flame has an oxidizing atmosphere, so this flame is suitable for the determination of alkali metal elements. Chemical Metering Flame is a stoichiometric relationship calculated fuel and oxidizer ratio combustion flame, it has a high temperature, less interference, stable, low background characteristics, in addition to alkali metals and easy to form elements of refractory oxides, most common elements commonly used this flame. Fu is the flame with excessive fuel, because the combustion is not complete, the flame has a strong reduction atmosphere, so, the flame has a reduction, suitable for the determination of more easily formed refractory oxides of elements such as molybdenum, rare earth elements.




Slit
When the measured elements have no adjacent interference lines, such as potassium, sodium, etc., can be used larger slit. When the measured elements have adjacent interference lines, such as calcium, iron, magnesium, etc., the smaller slit can be used. Several factors that affect the sensitivity are opposites. In the specific testing work, the inspectors should consider several factors, according to the instrument and the situation to adjust several factors to achieve the best working condition.






5.difference

The Flame photometer uses the atomic emission principle to make the corresponding substance atomized (a solid solution, such as: dissolved with acid. Liquid high temperature, gas used in the discharge of the excitation), the excited electrons are at high energy level, instability will jump back to the ground state, different levels of atomic electrons, the transition will emit different wavelengths of light waves, through the analysis of light waves will know what the atom. Similarly, the intensity of the light wave can be analyzed to determine the content of the atom. Such as:FPT-640The Flame photometer (usually factory-supplied with a potassium-sodium detector) is used to analyze potassium and sodium in the blood, and is also used in the analysis of the silicic acid industry. Ultraviolet-visible Spectrophotometer is the use of absorption principle, ultraviolet region (200-400generally used for the analysis of organic matter, some specific functional groups will have absorption (molecular absorption), often used to measure the amount of preservatives, usually with the maximum absorption of wavelength measurement, but there are a variety of material absorption, often used is a full sweep single sample, and then test the composite sample, take multipoint calculation, Can know the different substance content (this is a teacher's master's thesis oh); Visible area (400-760generally used for the analysis of ions, just like the general spectrophotometer such as:721type.






6.Impact Analysis

Flame Photometric analysis-Impact Factors1

1, excitation conditions:

1) Flame temperature: The temperature is too low sensitivity decreases, the temperature is too high, alkali metal ionization is serious, affecting

The linear relationship of the measurement.

Factors affecting the flame temperature:

-gas type: Using propane-Air, butane-Air or liquefied petroleum gas-air and other low temperature fire

Flame(about1900 ℃)more suitable and convenient

-gas and fuel gas ratio: maintain proper

-Sample Solution Suction: The flame temperature will drop when it is too large

2) Gas pressure: The gas pressure must be kept constant at the time of determination.

3Sprayer: Sprayer is not clean, easy to cause the test fluid atomization is bad, the test must be clear, and at any time with water or ethanol cleaning sprayer.

4The height of the liquid level: changes in the level of the liquid surface, will cause the concentration of the elements after the excitation changes, the test must be kept in high consistency.

Flame Photometric analysis-Impact Factors2

2, type and composition of specimen

1the ionization and self-absorption of the element can cause the correction curve to bend and the linear range to narrow. such as potassium at high concentrations of self-absorption is serious, so that the correction curve to the horizontal direction of bending, at low concentrations due to the increase in ionization, radiation enhancement, correction curve to the ordinate direction of bending.

2The co-ions in the specimen have an influence on the determination, such as the spectral line enhancement when the alkali metal coexist, and the result is high.

3) The physical properties of the specimen should be consistent with the composition of the standard solution

Flame Photometric analysis-Impact Factors3

3, instrument quality

1the selectivity of Monochromator: The filter is good quality, can reduce the interference of co-existence material.

2) The influence of the surrounding environment on the instrument.

3The light battery is used too long to produce fatigue.

7How to choose

A thermal analyzer is a type of instrument that uses a program to control the temperature of a substance by measuring its physical properties and temperature. It has been widely used in many fields such as production experiment. Most customers are at a loss when choosing a thermal analyzer and don't know how to choose the right model for themselves. Let's briefly introduce some of the parameters of the thermal analyzer.

First we know that thermal analyzers are some of the relationships between the physical and chemical properties of a substance and its temperature. So the temperature it can reach is one of our most concerned. Most of the thermal analyzers on the market are +more or more degrees Celsius. But there's a difference here. If the object to be tested for different materials, the required temperature is not the same. As we all know, the glass material is mostly silica, its melting point is generally1200 ℃around. Therefore, it is necessary1250 ℃about or even higher. But for some of the relative temperature requirements are lower, such as some calcium carbonate, calcium sulfate, such as rocks, most of the temperature in800 ℃about, choose1000 ℃of the Can.

Second, you need to choose which type. The market can be broadly divided into three kinds: differential heat type, hot heavy, comprehensive type. The differential heat type can be measured by the temperature, sensitivity, range and other parameters. Thermal heavy-duty can be measured for heat relive, sensitivity, range, etc. The comprehensive model combines the full performance of the above two, and can measure the thermal weight difference heat separately. When measuring some different properties of the sample, you need to select different types of instruments and consider the cost-performance ratio. Relatively speaking, the comprehensive cost-effective of course the highest, but also the first choice for many customers. Others, such as analytical method, are relative to their differential heat type, hot and heavy. Differential heat Type GeneralDTAtype of analysis, thermal heavy isTG-DTGtype.

Some other small influence parameters such as size, weight, etc., can be corresponding to the customer's own needs to choose, in general, of course, the lighter the smaller, convenient mobile first. These are some of the personal insights on thermal analyzers that are welcome to discuss.

FP64350 is an analytical instrument designed and manufactured in accordance with the basic principles of emission spectra.

Widely used in agricultural fertilizer, soil analysis, cement analysis, silicate industry analysis and determination;

Clinical laboratory and Pathological study of medical and health care, and have the ability to take lithium salt in psychiatric patients.

1. switch on the power supply, start the air compressor, insert the sample tube into distilled water, and soon in the waste dish there is the outflow of liquid, that is, the Flame photometer chamber works normally.

2. Open the gas valve and press the ignition button to open the gas valve gradually while pressing the ignition button.

3. after ignition, make the flame light blue, tapered and slightly curved at the bottom.

4. after the flame is normal, the instrument should be preheated for up to five minutes.

5. Calibrating the instrument with a standard solution at a concentration of μg / ml, so that the KandNa readings are "0".

6. Sample Determination: Insert the sample tube into the prepared specimen, and when the readings are stable, record the results.

7. after the test specimen is finished, it is still needed for 5 minutes to clean the instrument with distilled water .

8. shut down: First close the gas valve, after the flame extinguished, then close the instrument and air compressor switch.

9. after the shutdown, the instrument sampling switch, gas valve can not be spinning, still maintain the original state, so that the next boot ignition.

Operation of Flame Photometer

1.plug in the air compressor, start the air compressor, the visible pressure gauge is gradually rising. Pull up the air filter to reduce the adjustment knob, then turn the adjustment knob clockwise or counterclockwise, the pressure can be adjusted to0.15MPaaround. The pipette is inserted into the solution, the solution into the atomization chamber, and soon in the waste dish has a solution outflow, which means that the instrument into the normal atomization, the waste dish is decentralized a container, the collection of waste water is good.

2.plug in the host power cord, turn on the power switch, and then open the LPG cylinder on the switch, the gas valve to the appropriate position by the ignition button, and then from the observation window can see the ignition flower, rotary gas valve to adjust the flame height, so that the flame appears blue cone Flame, the instrument into the preheating. If there's no fire, the instrument shows.Err1, can increase the opening of the gas valve, and then press the ignition button from the new ignition. The sound and light alarm will be displayed in use due to gas exhausted or other reasons.ERR2and automatically shut off the gas solenoid valve, to prevent gas benefits.



3.The combustion of the flame and the injection of the sample is a dynamic process. At first, it is at room temperature, then the heating process, when the gas and sample quantity are determined. The flame tends to heat balance, when the flame is stable and the energy is constant, so the readings are stable.



4.warm-up time is more necessary -minutes, the use of distilled water continuous injection is good, because it is more able to simulate the actual injection conditions.



5.when the power off, the liquefied petroleum gas cylinders are closed (clockwise tightening), the residual LPG in the pipeline after burning, the flame goes out. Before shutting down, please use distilled air to burn5minute or so. After the shutdown, the instrument of the gas valve can not be compared to Rotary, the next use just open the switch on liquefied petroleum gas cylinders at the same time by the ignition switch, the flame state is no better than the adjustment, gas open, close another solenoid valve control.
When the fire point is not, you can increase the amount of gas, and then adjust after the point.

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Flame Spectrophotometer FP64350 Operating Procedures