CN1036418C - Flame atomic absorption spectrometry - Google Patents
Flame atomic absorption spectrometry Download PDFInfo
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- CN1036418C CN1036418C CN92101560A CN92101560A CN1036418C CN 1036418 C CN1036418 C CN 1036418C CN 92101560 A CN92101560 A CN 92101560A CN 92101560 A CN92101560 A CN 92101560A CN 1036418 C CN1036418 C CN 1036418C
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Abstract
The present invention belongs to flame atomic absorption spectrum technique which adopts a method of oxygen enriched air acetylene flame and a special flame atomization device and overcomes the defects of low temperature and sensitivity, few species of analysis elements, toxic nitrous oxide acetylene flame, high cost, non controllable and adjustable flame, etc. of the existing air acetylene flame method widely applied. Thus, the present invention is suitable for analyzing and testing most of elements in any field.
Description
The invention belongs to atomic absorption spectroscopy
Flame atomic absorption spectrometry is a kind of instrument analytical method simple to operation, is widely used in the assay determination of various elements of every field such as geology, metallurgy, chemical industry, medicine, biology, environmental protection.
The flame atomic absorption spectrometry of using mainly contains two classes at present: a class is an air-acetylene flame, this class flame only is 21% owing to containing oxygen in the combustion air, therefore temperature is lower, be 2600K, most of elements evaporate disassociation not exclusively under this temperature, atomization efficiency is low, so be only applicable to the oxide dissociation energy less than 5ev and fusing point, some elements that boiling point is lower, as alkaline metal, copper divides family, zinc divides family, iron, cobalt, nickel, elements such as manganese, dissociate into 5-ev for oxide, fusing point, some elements that boiling point is slightly high are as earth alkali metal, chromium, molybdenum, measurement sensitivities such as gallium are lower, and chemical serious interference; For the oxide dissociation energy greater than 6ev, fusing point, the element that boiling point is higher can almost can't be measured by element as aluminium, rare earth, titanium, zirconium, vanadium, niobium, tungsten, silicon.Another kind of is nitrous oxide acetylene torch (J.B.Willis, Nature, 1965,207,715), this class flame at high temperature dissociates and emits oxygen, oxygen level reaches 33%, and in disassociation release heat, so temperature is higher, reach 3200K, for dissociation energy is 5-6ev and greater than 6ev, and fusing point, the element that boiling point is high almost can both be measured, still, nitrous oxide is a kind of toxic gas, cost height (every bottle about 500 yuan), air consumption is big, is difficult for buying, can not usually select best probe temperature according to different units during operation, be subjected to great restriction in the use.
Except above-mentioned two classes flame, there is the people once to test pure oxygen acetylene torch and nitrogen oxyacetylene torch (M.D.Amos, P.E.Thomas, Anal.Chim.Acta, 1965,32,139 for application in analyzing; M.D.Amos, J.B.Willis, Spectrochim, Acta, 1966,22,1325).Though the temperature of these two kinds of flames also can be up to 3200K, but its burning rate is very fast, particularly very easily produce tempering greater than 60% the time and set off an explosion when oxygen level in the combination gas, the air-acetylene flame that Ke Ke Bright (Kirkbright) once studied with oxygen shielding once took place and prevented to produce tempering in this accident, but the temperature of this flame can only reach 2900K, and flame fluctuation, noise is big, performance can not show a candle to the nitrous oxide acetylene torch, for this reason, on existing commercial flame atomization device, usually obviously mark the printed words of " the inaccurate oxygen that uses ".
The oxygen-enriched air acetylene torch atomic absorption spectrography (AAS) and the special-purpose flame atomization device thereof that the purpose of this invention is to provide a kind of safe high temperature.
Improving the sensitivity of flame atomic absorption spectrometry and reducing the chemical key of disturbing is to improve the temperature of flame, and the key that improves flame temperature mainly is to depend on the content that improves oxygen in acetylene gas and the combustion-supporting gas, and the flow of the random regulating and controlling all gases component of energy.
The present invention adopts and add purity oxygen in air, make it become oxygen-enriched air, be mixed into the oxygen-enriched air acetylene torch with acetylene gas again, and by flowmeter control air, the flow of oxygen and acetylene gas, the tested element of difference is selected best flame status, design the flame atomization device of special-purpose safety simultaneously for this oxygen-enriched air acetylene torch.
The special-purpose flame atomization device of oxygen-enriched air acetylene torch method of the present invention is made of air path part, sprayer, imbibition kapillary, waste liquid outlet, impact bead, mixing chamber, burner and explosion-protection equipment of preventing tempering etc.Wherein, air path part has increased the oxygen gas circuit; The material of mixing chamber can be steel, interior enamel coating, fluoroplastic or other engineering plastics; Combustion head can also attach water cooling plant with the single seam stainless steel of 0.5 * 100mm or the burner of titanium system; Explosion-protection equipment is made of critical pieces such as plastic sheeting, spring, rubber collars, and guaranteeing can provide unimpeded passage to compressed air stream when causing tempering owing to operating mistake.
Use the flame atomization device of special use of the present invention, oxygen-enriched air acetylene torch method can be controlled enforcement by following four kinds of methods:
1. increase an oxygen gas circuit in the flame atomization device of double air road system, this gas circuit is entered mixing chamber and is controlled its flow respectively with flowmeter by the sprayer gas circuit with after pressure air gas circuit is mixed by three-way pipe.
2. the oxygen gas circuit is introduced from former auxiliary air gas circuit in the flame atomization device of three air-channel systems, and controls its flow respectively with flowmeter.
3. increase an oxygen gas circuit in the flame atomization device of three air-channel systems, this gas circuit and auxiliary air gas circuit are mixed after by three-way pipe, enter mixing chamber by the auxiliary air gas circuit, and control its flow velocity respectively with flowmeter.
4. the flame atomization device of one four air-channel system promptly in original sprayer air gas circuit, increases an oxygen gas circuit on the basis of auxiliary air gas circuit and acetylene gas gas circuit.
The temperature of oxygen-enriched air acetylene torch burning of the present invention can be up to 3200K, can also be by controlling oxygen easily, the flow of air and acetylene gas is selected best flame status to the analyzed element of difference, therefore can be widely used in analyzing the oxide dissociation energy less than 5ev, 5ev-6ev reaches greater than 6ev and fusing point and the higher most of elements of boiling point, compare with nitrous oxide acetylene torch method, the highly sensitive 2-10 of oxygen-enriched air acetylene torch method is (seeing Table 1) doubly, can remove separation and concentration step to tested sample, simple to operation, with low cost, safety non-toxic.The special-purpose flame atomization device construction of oxygen-enriched air acetylene torch method is simple, material is not overcritical, flexible to operation, safe and reliable, very easily change into the oxygen-enriched air acetylene torch, and flameholding table 1 has been listed the correlation data that air-acetylene flame, nitrous oxide acetylene torch and oxygen-enriched air acetylene torch are analyzed the sensitivity of some element from air-acetylene flame.(table is seen the literary composition back)
Drawing explanation accompanying drawing 1. has oxygen gas circuit and air gas circuit to constitute the special-purpose flame atomization installation drawing of oxygen-enriched air acetylene torch method of the double air road system that mixes gas circuit.
The special-purpose flame atomization installation drawing of the oxygen-enriched air acetylene torch method of three air-channel systems that accompanying drawing 2. oxygen gas circuits are introduced from former auxiliary air gas circuit.
Accompanying drawing 3. has oxygen gas circuit and air gas circuit to constitute the special-purpose flame atomization installation drawing of oxygen-enriched air acetylene torch method of three air-channel systems that mix gas circuit.
The special-purpose flame atomization installation drawing of the oxygen-enriched air acetylene torch method of accompanying drawing 4. 4 air-channel systems.
Embodiment 1
In double air road system flame atomization device shown in Figure 1, oxygen is introduced by oxygen gas circuit (9), air is introduced by air gas circuit (10), both mix through three-way pipe, enter mixing chamber (2) by the sprayer (5) that imbibition kapillary (7) are housed again, acetylene gas is introduced mixing chamber (2) by acetylene gas gas circuit (8), lights on burner (1) at last, impact bead (4) and explosion-protection equipment (3) are housed in the mixing chamber (2), and waste liquid is discharged from waste liquid outlet (6).On the basis that guarantees nebulization efficiency, the flow that enters the combination gas of mixing chamber (2) from sprayer (5) should reach 7L/min to 10L/min, just has enough big unburned gas flow velocity to protect, and prevents tempering.In the spraying of this mixing, along with the increase of oxygen flow in the combination gas, air mass flow reduces accordingly, can calculate oxygen level in this combination gas according to the ratio of its flow; The flow maximum of acetylene gas should reach 10L/min to 12L/min.All should under little rich combustion or rich combustion condition (reducing atmosphere), carry out most elements during use.Can light flame with air acetylene condition earlier, increase the acetylene flow later on gradually, and corresponding increase oxygen flow.Under this little rich combustion or rich combustion condition, when flame temperature increases the experiment end with the increase of acetylene gas flow, should close the oxygen gas circuit earlier, close the acetylene gas circuit more gradually, must keep flame to be in fuel-rich state forever.
In three air-channel system flame atomization devices shown in Figure 2, oxygen directly enters mixing chamber (2) by oxygen gas circuit (9), air is entered by air gas circuit (10) and enters mixing chamber (2) other parts behind the sprayer (5) again and be adjusted in 5-10L/mim with spray air flow (I) in embodiment 1 sprayer (5), have higher nebulization efficiency oxygen flow (F) scope at 0＜F＜6L/min with assurance, and accurate adjustable.The introducing of oxygen does not influence the flow of spray air in this device, and the flow of acetylene gas (II) maximum should reach 10L/min to 12L/min.Use method of operating with embodiment 1.
In three air-channel system flame atomization devices shown in Figure 3, oxygen is introduced by oxygen gas circuit (9), auxiliary air is introduced by auxiliary air gas circuit (11), both directly enter mixing chamber (2) after three-way pipe mixes, other parts are with embodiment 2, auxiliary air flow (G) scope is at 0＜G＜10L/min, and the increase of auxiliary air reduces oxygen content in the combination gas to improve flame height.Other gas flow scope is with embodiment 2.Use method of operating with embodiment 1.
In four air-channel system flame atomization devices shown in Figure 4, oxygen directly enters mixing chamber (2) by oxygen gas circuit (9), auxiliary air is directly introduced mixing chamber (2) by auxiliary air gas circuit (11), other parts are with embodiment 2, the all gases flow range uses method of operating with embodiment 1 with embodiment 3.
The mensuration of ytterbium is used double air road system flame atomization device shown in Figure 1, air mass flow 5.13L/min, oxygen flow 2.20L/min.Acetylene air-flow 5.83L/min, flame height 6mm, combination gas oxygen level 45%, O
2/ C
2H
2=0.56, little rich combustion, Yb398.8nm, characteristic concentration are 0.025 μ g/ml (containing 0.1%Kcl and 1% sulfosalicylic acid).
Embodiment 6
The mensuration of europium is used double air road system flame atomization device shown in Figure 1, air mass flow 5.33L/min, oxygen flow 2.00L/min.Acetylene flow 5.50L/min, flame height 6mm, combination gas oxygen level 42%, O
2/ C
2H
2=0.57, little rich combustion, Eu459.4nm, characteristic concentration are 0.08 μ g/ml (containing 0.1%Kcl and 1% sulfosalicylic acid)
The mensuration of aluminium is used double air road system flame atomization device shown in Figure 1, air mass flow 4.70L/min, oxygen flow 2.60L/min.Acetylene gas flow 7.00L/min, flame height 8mm, combination gas oxygen level 49%, O
2/ C
2H
2=0.54, rich combustion, Al309.2nm, characteristic concentration are 0.3 μ g/ml.
The mensuration of molybdenum is used three air-channel system flame atomization devices shown in Figure 3, air mass flow 6L/min, acetylene gas flow 5.5L/min, auxiliary air flow 2.5L/min, oxygen flow 1.8L/min.Mix combustion-supporting gas oxygen level 35%,, oxycetylene is than 0.65, and richness is fired, Mo313.3nm10mA, characteristic concentration 0.15 μ g/ml.
The mensuration of tungsten, use three air-channel system flame atomization devices shown in Figure 3, air mass flow 6L/min, acetylene gas flow 6L/min, auxiliary air flow 2.5L/min, oxygen flow 1.8L/min mixes combustion-supporting gas oxygen level 35%, oxycetylene is than 0.60, Fu Ran, W255.1nm12mA, characteristic concentration 3.2 μ g/ml.
The mensuration of samarium, use three air-channel system flame atomization devices shown in Figure 3, air mass flow 6L/min, acetylene gas flow 8.5L/min, auxiliary air flow 5L/min, oxygen flow 3.7L/min mixes combustion-supporting gas oxygen level 41%, oxycetylene is than 0.70, little rich combustion, Sm429.6nm9mA, characteristic concentration 2.3 μ g/ml.
Table 1
Flame status air acetylene nitrous oxide oxygen-enriched air element flame acetylene torch acetylene torch Ca characteristic concentration 0.07 0.05 0.008 Mg (μ g/ml) 0.007-0.003 Yb 7.6 0.08 0.025 Eu 3 0.3 0.08 Al-0.7 0.3 Sr 0.15 0.1 0.015 Ba 10 0.4 0.1 Mo 0.8 0.4 0.15 W-5 3.2 Ga 1.3 1.0 0.4 Sm-8.5 2.3 La-35 20
Claims (10)
1. flame atomic absorption spectrometry art, it is characterized in that: adopt in air, to add purity oxygen, be mixed into the oxygen-enriched air acetylene torch with acetylene gas again, it is as follows to control the flow of air, oxygen and acetylene gas by flowmeter when analyze using, the scope of introducing purity oxygen flow (F) is 0＜F＜6L/min, the scope of auxiliary air flow (G) is 0＜G＜10L/min, and acetylene gas flow (H) maximal value is 4.7L/min＜I＜10L/min in the scope of 10L/min to 12L/min spray air flow (I).
2. according to the described flame atomic absorption spectrometry art of claim 1, it is characterized in that adopting two gas circuit air supply methods, wherein oxygen is introduced by oxygen gas circuit (9), air is introduced by air gas circuit (10), both mix through three-way pipe, enter mixing chamber (2) by the sprayer (5) that imbibition kapillary (7) are housed again, acetylene gas is introduced mixing chamber (2) by acetylene gas gas circuit (8), after air and oxygen mix in mixing chamber (2), light in burner (1) top at last, the gas flow of each gas circuit is controlled with flowmeter respectively.
3. according to the described flame atomic absorption spectrometry art of claim 1, it is characterized in that adopting three gas circuit air supply methods, wherein oxygen enters mixing chamber (2) by oxygen gas circuit (9), air enters mixing chamber (2) by air gas circuit (10) by the sprayer (5) that imbibition kapillary (7) are housed, acetylene gas is introduced mixing chamber (2) by acetylene gas gas circuit (8), after these three kinds of gases mix in mixing chamber (2), light in burner (1) top, the gas flow of each gas circuit is controlled with flowmeter respectively.
4. according to the described flame atomic absorption spectrometry art of claim 1, it is characterized in that adopting three gas circuit air supply methods, wherein oxygen is introduced by oxygen gas circuit (9), auxiliary air is introduced by auxiliary air gas circuit (11), these two kinds of gases enter mixing chamber (2) again after three-way pipe mixes, air enters mixing chamber (2) by air gas circuit (10) by the sprayer (5) that imbibition kapillary (7) are housed, acetylene gas is introduced mixing chamber (2) by acetylene gas gas circuit (8), after these four kinds of gases mix in mixing chamber (2), light in burner (1) top, the gas flow of each gas circuit is controlled with flowmeter respectively.
5. according to the described flame atomic absorption spectrometry art of claim 1, it is characterized in that adopting four gas circuit air supply methods, wherein oxygen is introduced mixing chamber (2) by oxygen gas circuit (9), auxiliary air is introduced mixing chamber (2) by auxiliary air gas circuit (11), air enters mixing chamber (2) by air gas circuit (10) by the sprayer (5) that imbibition kapillary (7) are housed, acetylene gas is introduced mixing chamber (2) by acetylene gas gas circuit (8), after these four kinds of gases mix in mixing chamber (2), light in burner (1) top, the gas flow of each gas circuit is controlled with flowmeter respectively.
6. flame atomization device that flame atomic absorption spectrometry art as claimed in claim 1 is used, by sprayer (5), imbibition kapillary (7), waste liquid outlet (6), impact bead (4), mixing chamber (2), burner (1), the explosion-protection equipment (3) and the air path part that prevent tempering are formed, and it is characterized in that air path part is by oxygen gas circuit (9), air gas circuit (10), constitute with acetylene gas gas circuit (8), or by oxygen gas circuit (9), air gas circuit (10), acetylene gas gas circuit (8) and auxiliary air gas circuit (11) are formed, the acetylene gas gas circuit is connected on the mixing chamber (2), oxygen gas circuit (9) is connected on sprayer (5) and goes up or be connected on the mixing chamber (2), and the air gas circuit is connected on the sprayer (5), and the auxiliary air gas circuit is connected on the mixing chamber (2).
7. according to the described flame atomization device of claim 6, it is characterized in that oxygen gas circuit (9) is connected with sprayer (5) by three-way pipe with air gas circuit (10), acetylene gas gas circuit (8) is connected with mixing chamber (2).
8. according to the described flame atomization device of claim 6, it is characterized in that oxygen gas circuit (9) is connected with mixing chamber (2), air gas circuit (10) is connected with sprayer (5), and acetylene gas gas circuit (8) is connected with mixing chamber (2).
9. according to the described flame atomization device of claim 6, it is characterized in that oxygen gas circuit (9) is connected with mixing chamber (2) by three-way pipe with auxiliary air gas circuit (11), air gas circuit (10) is connected with sprayer (5), and acetylene gas gas circuit (8) is connected with mixing chamber (2).
10. according to the described flame atomization device of claim 6, it is characterized in that oxygen gas circuit (9), auxiliary air gas circuit (11), acetylene gas gas circuit (8) directly is connected with mixing chamber (2) respectively, and air gas circuit (10) is connected with sprayer (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92101560A CN1036418C (en) | 1992-03-09 | 1992-03-09 | Flame atomic absorption spectrometry |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92101560A CN1036418C (en) | 1992-03-09 | 1992-03-09 | Flame atomic absorption spectrometry |
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| Publication Number | Publication Date |
|---|---|
| CN1076278A CN1076278A (en) | 1993-09-15 |
| CN1036418C true CN1036418C (en) | 1997-11-12 |
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| CN92101560A Expired - Fee Related CN1036418C (en) | 1992-03-09 | 1992-03-09 | Flame atomic absorption spectrometry |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100356161C (en) * | 2004-12-27 | 2007-12-19 | 郴州钻石钨制品有限责任公司 | Rapid analysis and detection method for tin element in tungsten smelting |
| US20120150451A1 (en) * | 2010-12-13 | 2012-06-14 | Halliburton Energy Services, Inc. | Optical Computation Fluid Analysis System and Method |
| CN102680454B (en) * | 2011-09-20 | 2014-06-18 | 深圳市爱诺实业有限公司 | Second-order differential flame emission spectrometer |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3520406A1 (en) * | 1984-06-08 | 1985-12-12 | Hitachi, Ltd., Tokio/Tokyo | Flame atomic absorption spectrophotometer |
| CN85108149A (en) * | 1984-11-13 | 1986-08-27 | 珀金·埃尔默有限公司 | The safety feature of atomic absorption spectrophotometer burner |
| CN85108151A (en) * | 1984-11-13 | 1986-09-03 | 珀金·埃尔默有限公司 | Be used for improvement system at flame atomic absorption spectrophotometer conversion oxygenant |
| SU1497528A1 (en) * | 1987-06-30 | 1989-07-30 | Тбилисское Научно-Производственное Объединение "Аналитприбор" | Method of atomic-absorption analysis of substances |
-
1992
- 1992-03-09 CN CN92101560A patent/CN1036418C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3520406A1 (en) * | 1984-06-08 | 1985-12-12 | Hitachi, Ltd., Tokio/Tokyo | Flame atomic absorption spectrophotometer |
| CN85108149A (en) * | 1984-11-13 | 1986-08-27 | 珀金·埃尔默有限公司 | The safety feature of atomic absorption spectrophotometer burner |
| CN85108151A (en) * | 1984-11-13 | 1986-09-03 | 珀金·埃尔默有限公司 | Be used for improvement system at flame atomic absorption spectrophotometer conversion oxygenant |
| SU1497528A1 (en) * | 1987-06-30 | 1989-07-30 | Тбилисское Научно-Производственное Объединение "Аналитприбор" | Method of atomic-absorption analysis of substances |
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| CN1076278A (en) | 1993-09-15 |
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