CN1076278A - Flame atomic absorption spectrometry - Google Patents
Flame atomic absorption spectrometry Download PDFInfo
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- CN1076278A CN1076278A CN 92101560 CN92101560A CN1076278A CN 1076278 A CN1076278 A CN 1076278A CN 92101560 CN92101560 CN 92101560 CN 92101560 A CN92101560 A CN 92101560A CN 1076278 A CN1076278 A CN 1076278A
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- gas circuit
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- acetylene
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Abstract
The invention belongs to the flame atomic absorption spectrometry art, adopt oxygen-enriched air acetylene torch method and special-purpose flame atomization device thereof, the air-acetylene flame method temperature that has overcome present widespread use is low, sensitivity is low, but the analytical element kind is few and the nitrous oxide acetylene torch is poisonous, cost height, flame can not regulating and controlling etc. shortcoming, therefore be applicable to the analytical test of the most of elements in the every 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.One 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, divides elements such as family, iron, cobalt, nickel, manganese as alkaline metal, copper branch family, zinc; For the oxide dissociation energy is 5-6ev, and some elements that fusing point, boiling point are slightly high are lower as measurement sensitivities such as earth alkali metal, chromium, molybdenum, galliums, and chemical serious interference; Greater than 6ev, fusing point, the element that boiling point is higher almost can't be measured as elements such as aluminium, rare earth, titanium, zirconium, vanadium, niobium, tungsten, silicon for the oxide dissociation energy.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, its burning rate is very fast, particularly very easily produces tempering when oxygen level in the combination gas greater than 60% the time and sets off an explosion, and this accident once took place.The air-acetylene flame that Ke Ke Bright (Kirkbright) was once studied with the oxygen shielding prevents to produce tempering, but the temperature of this flame can only reach 2900K, and the flame fluctuation, and noise is big, and 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 the flow by flowmeter control air, 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, gas circuit has partly 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 the separation and concentration step to tested sample from, and is 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 changes into the oxygen-enriched air acetylene torch from air-acetylene flame, 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.
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 (μg/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
The 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, to guarantee having enough big unburned gas flow velocity, 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, flame temperature increases with the increase of acetylene gas flow.When experiment finishes, should close the oxygen gas circuit earlier, close the acetylene gas circuit more gradually, must keep flame to be in fuel-rich state forever.
Embodiment 2
In three air-channel system flame atomization devices shown in Figure 2, oxygen directly enters mixing chamber (2) by oxygen gas circuit (9), and air enters mixing chamber (2) other parts again with embodiment 1 after entering sprayer (5) by air gas circuit (10).Spray air flow (I) is adjusted in 5-10L/min in the sprayer (5), to guarantee to have higher nebulization efficiency.Oxygen flow (F) scope is at 0＜F≤6L/min, and precision is adjustable.The introducing of oxygen does not influence the flow of spray air in this device.The flow of acetylene gas (H) maximum should reach 10L/min to 12L/min.Use method of operating with embodiment 1.
Embodiment 3
In three air-channel system flame atomization devices shown in Figure 3, oxygen is introduced by oxygen gas circuit (9), and auxiliary air is introduced by auxiliary air gas circuit (11), and both directly enter mixing chamber (2) after three-way pipe mixes, and 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.
Embodiment 4
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), and other parts are with embodiment 2, and all gases flow range is with embodiment 3.Use method of operating with embodiment 1.
Embodiment 5
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 gas 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 that 0.025 μ g/ml(contains 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 that 0.08 μ g/ml(contains 0.1%KCl and 1% sulfosalicylic acid).
Embodiment 7
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, Al 309.2nm, characteristic concentration are 0.3 μ g/ml.
Embodiment 8
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 mixes combustion-supporting gas oxygen level 35%, and oxycetylene is than 0.65, and richness is fired, Mo313.3nm 10mA, characteristic concentration 0.15 μ g/ml.
Embodiment 9
The mensuration of tungsten is used 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%, and oxycetylene is than 0.60, and richness is fired, W255.1nm12mA, characteristic concentration 3.2 μ g/ml
Embodiment 10
The mensuration of samarium is used 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%, and oxycetylene is than 0,70, and little richness is fired Sm 429.6nm9mA, characteristic concentration 2.3 μ g/ml
Claims (12)
1, a kind of flame atomic absorption spectrometry art is characterized in that: adopt oxygen-enriched air acetylene torch method.
2, according to the described oxygen-enriched air acetylene torch of claim 1 method, it is characterized in that: 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, the maximum scope of acetylene gas flow (H) is 10≤H≤12L/min, and the range regulation of spray air flow (I) is at 5≤I≤10L/min.
3, according to the described oxygen-enriched air acetylene torch of claim 1 method, it is characterized in that: the flow of all gases component can carry out arbitrarily and accurate adjusting according to the needed best flame temperature of analyzed element.
4, according to the described oxygen-enriched air acetylene torch of claim 1 method, it is characterized in that it being two gas circuit air supply methods, comprise by what oxygen gas circuit (9) and air gas circuit (10) were formed and mix gas circuit and acetylene gas gas circuit (8), every gas circuit is used flowmeter pilot-gas flow respectively.
5, according to the described oxygen-enriched air acetylene torch of claim 1 method, it is characterized in that it being three gas circuit air supply methods, comprise by what oxygen gas circuit (9) or oxygen gas circuit (9) and auxiliary air gas circuit (11) were formed and mix gas circuit, air gas circuit (10) and acetylene gas gas circuit (8), every gas circuit is used flowmeter pilot-gas flow respectively.
6, according to the described oxygen-enriched air acetylene torch of claim 1 method, it is characterized in that it being four gas circuit air supply methods, comprise oxygen gas circuit (9), auxiliary air gas circuit (11), air gas circuit (10) and acetylene gas gas circuit (8), every gas circuit is used flowmeter pilot-gas flow respectively.
7, the special-purpose flame atomization device of the described method of a kind of claim 1 is characterized in that: be provided with the oxygen gas circuit, can use oxygen.
8, according to the described special-purpose flame atomization device of claim 7, it is characterized in that: in the flame atomization device of double air road system, increase an oxygen gas circuit (9), this gas circuit (9) is with after pressurized air gas circuit (10) is mixed by three-way pipe, enter mixing chamber (2) by sprayer (5) gas circuit, be equipped with flowmeter on each bar gas circuit.
9, according to the described special-purpose flame atomization device of claim 7, it is characterized in that: oxygen gas circuit (9) is introduced from former auxiliary air gas circuit in the flame atomization device of three air-channel systems, is equipped with flowmeter on each bar gas circuit.
10, according to the described special-purpose flame atomization device of claim 7, it is characterized in that: in the flame atomization device of three air-channel systems, increase an oxygen gas circuit (9), this gas circuit (9) is mixed the back with auxiliary air gas circuit (11) by three-way pipe and is directly introduced mixing chamber (2), is equipped with flowmeter on each bar gas circuit.
11, according to the described special-purpose flame atomization device of claim 7, it is characterized in that: the atomizing apparatus that is one four air-channel system, promptly include oxygen gas circuit (9) pressurized air gas circuit (10), auxiliary air gas circuit (11) and acetylene gas gas circuit (8), (8), (9), (11) all directly introduce mixing chamber (2), are equipped with flowmeter on each bar gas circuit.
12, according to the described special-purpose flame atomization device of claim 7, it is characterized in that: the explosion-protection equipment (3) that prevents tempering is housed in mixing chamber (2).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92101560A CN1036418C (en) | 1992-03-09 | 1992-03-09 | Flame atomic absorption spectrometry |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92101560A CN1036418C (en) | 1992-03-09 | 1992-03-09 | Flame atomic absorption spectrometry |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1076278A true CN1076278A (en) | 1993-09-15 |
| CN1036418C CN1036418C (en) | 1997-11-12 |
Family
ID=4939190
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN92101560A Expired - Fee Related CN1036418C (en) | 1992-03-09 | 1992-03-09 | Flame atomic absorption spectrometry |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102680454A (en) * | 2011-09-20 | 2012-09-19 | 深圳市爱诺实业有限公司 | Second-order differential flame emission spectrometer |
| CN103958831A (en) * | 2011-12-13 | 2014-07-30 | 哈里伯顿能源服务公司 | Optical computation fluid analysis system and method |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60262044A (en) * | 1984-06-08 | 1985-12-25 | Hitachi Ltd | Flame type atomic absorption spectrometer |
| US4568267A (en) * | 1984-11-13 | 1986-02-04 | The Perkin-Elmer Corporation | Safety apparatus for an atomic absorption spectrophotometer burner |
| US4571172A (en) * | 1984-11-13 | 1986-02-18 | The Perkin-Elmer Corporation | System for changing oxidants in a flame atomic absorption spectrophotometer |
| 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
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102680454A (en) * | 2011-09-20 | 2012-09-19 | 深圳市爱诺实业有限公司 | Second-order differential flame emission spectrometer |
| 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 |
| CN103958831A (en) * | 2011-12-13 | 2014-07-30 | 哈里伯顿能源服务公司 | Optical computation fluid analysis system and method |
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| Publication number | Publication date |
|---|---|
| CN1036418C (en) | 1997-11-12 |
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| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
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Granted publication date: 19971112 Termination date: 20100309 |