CN101319992A - Software for non-standard analysis of Zeeman background graphite furnace atomic absorption photometer - Google Patents
Software for non-standard analysis of Zeeman background graphite furnace atomic absorption photometer Download PDFInfo
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Abstract
Non-standard analyzing software in a Zeeman button background graphite furnace atom absorption photometer of the invention comprises: (I) software A which comprises table 1; (1) A1 secondary software; the aim is to work out the emendation coefficient K which is equal to m0exp<*>/m0exp, No.1 and No.2 demarcated solution in table 3-6 are used, and at the time, QA,0 is equal to the value of QA, and K is equal to m0exp<*>QAR<Z<PM>/0.0044m (formula 1-4); (2) A2 secondary software; the aim is to work out the turning value Ar of Zeeman standard curve; the QA value of No. 5 or 6 demarcated solution is used; (3) A3 software; the aim is to work out the bending coefficient Beta of the Zeeman standard curve; No. 3, No. 4 and No. 5 demarcated solution are used to work out Beta; (a) A3, 1 sub software; formula 5 and 6 are used to work out the corresponding values QA, 0 of No.3, 4 and 5 solution; (b) A3, 2subsoftware; table 2 is included; the corresponding value QA,0 of every QA at different Ar and different Beta is listed; (c) A3, 3 sub software; an inner insertion method is used as is shown in table 7, and formulas 7-9 are used to work out the value of Beta; (II) Beta software; the software A is used for working out the values of Ar and Beta (Y); the QA, 0 (X, Beta (Y)) value is worked out through the measured QA(X) value after the linearization; the inner insertion method shown in table 7 and formulas 10-12 are used for working out the QA, 0 (X, Beta (Y)) value; (III) C software; non-standard analyzing method basic formulas 13 and 14 are used for measuring the content m(pg) value of elements to be measured; (IV) software D; the software C is used for obtaining m value, and formula 15 is used for imputing the injection volume Mu1 of a solution sample or formula 16 is used for imputing the injection amount mg of a solid sample. The concentration C is worked out. The solution is pg/Mu1. The solid is the value of pg divided by mg.
Description
The design basis of the software that no standard analysis is used in the Zeeman deduction background graphite furnace atomic absorption photometer is a basis, patent " no standard analysis with fixed metal tungsten or tantalum platform graphite furnace atomic absorption photometer " (application number 200710097221.5, April 29 2007 applying date).Easy for narrating, Zeeman deduction background is called for short Z, and graphite furnace atomic absorption photometer is GFAAS, is collectively referred to as ZGFAAS, and no standard analysis is STLA, and fixed metal tungsten or tantalum platform are WTaPGT, and software is RJ, and analytic curve is AQX, and integration is absorbed as Q
A, peak absorbance is A
p, analytical element content is m (pg), the test feature amount is m
0Exp, best m
0Exp is m
0Exp
*
During with the ZGFAAS analytic sample, Q
AThe analytic curve of-m (pg) is seriously crooked, must analyze with a plurality of standard solution, and this is to think for a long time to be difficult to realize the STLA one of the main reasons.Must be with the Q that measures
AObtain meeting the Q of linearization requirement through linearization process
A, 0, just might carry out STLA.And to realize the linearization requirement, just must carry out scrutiny to the crooked source of analytic curve.This itself is exactly long-term complicated system engineering.The present inventor is a small-sized graphite furnace of using commodity HGA type (graphite pipe range 28mm, internal diameter 6mm, external diameter 8mm) invention in promptly 1972 at home and abroad on the document the earliest, than the HGA74 type of PE company Zao 2 years, carry out 53 elements A QX researchs (happy year of horse, environmental science reference 1976, (2); 18).The present inventor was developed into D in 1972
2Lamp is buckled background GFAAS, the persuasion leader of second optical instrument factory, Beijing (northern two light), apply for 200,000 yuan to the State Scientific and Technological Commission, participate in circuit and digital demonstration work with instrument cost persuasion Beijing mining and metallurgy institute, succeeding in developing Chinese first Tianwan businessman's product GFAAS in 1975 is the WFD-Y3 type, 70 units participate in evaluation meeting and think that small-sized graphite furnace is world lead level (than Zao 2 years of the HGA74 of PE), and WFD-Y3 gets Chinese first national scientific award (1978 national science and technology conferences prize).Common graphite pipe (GT) (1971) and the pyrolysis coating graphite-pipe (PGT) (1977) invented the earliest with the present inventor.The present inventor finds that AQX is early crooked to 0.2 beginning, and each element bending is widely different, but common feature is arranged, and promptly m (pg) platform A occurs to AQX to a certain degree greatly
rValue is pressed B.V.L ' vov (Atomic Absorption Spectrochemicalanalysis, Adam Hilger LTD, 1970) theory, gets formula (a), α=(10
Ar-1)
-1(a), α=I/I in formula (a)
0(b) L ' vov thinks α I
0For the empty cathode modulation width of cloth that the slit bandwidth enters is penetrated light or is entered adjacent threads.The present inventor finds α I when debugging WFD-Y3
0Also be included in all optics of discovery in the debug process, the imperfection of monochromator and circuit and element, the present inventor is defined as the nonlinear factor that the instrument imperfection causes with α.Any raising enters photomultiplier luminous energy way (being that energy determines all), as reduce lens and catoptron, and shorten light path, improve the gratings strips number, dwindle monochromator, the high photomultiplier that amplifies low noise, the width of cloth that occurs when reducing atomization is penetrated noise, the empty cathode lamp of more important raising energy, therefore on the WFD-Y3 instrument, add 1: 5 empty cathode modulation power supply of pulse power supply, the raising of lamp energy does not increase the emission line self-priming again more than 5 times, makes α reduce to 0.001-0.003, A
rBring up to 2.5-3.0.If influenced by α, linearity can be up to 0.8A
r, i.e. 2-2.4.But in fact just begin bending more than 0.2, therefore be not enough to resolve crooked reason with α.
Another causes crooked reason is that the hyperfine structure (hfs) of lamp emission line is as υ Ag328.1, Al309.3, Au242.8, Ba553.5, Bi306.8,223.1, Cd228,8, Cs852.1, Cu324.8, Eu459.4, Ga287.4, Hg253.7, In303.9, K766.5, Li670.8, Mg285.2, Mn279.5, Na589.0, Pb283.3, Rb780.0, Sb217.6, Sn286.3, Te214.3, Tl276.8, Zn213.9, B249.7, C240.7, Os290.9,27 elements, its hfs separation delta υ
Kfa/ Δ υ
LGreater than 2, Δ υ
LBe the pressure broadening of lamp emission line, Δ υ
KfaGreater than 0.2cm
-1, L ' vov (the same) shows the bending that may cause with chart, but this influence is only arrived 0.6A to linearity
r, i.e. 1.5-2.Therefore use Δ υ
KfaBe not enough to resolve crooked reason equally.
Since 1976, L ' vov took to comprehensively commodity HGA graphite furnace AAS is transformed into the instrument that can be used to not have standard analysis, the 6th international spectrum meeting (1976, VI CSI.Philadelphia) be published in (Zh.Prikl.spektrosk.27,395 (1977), SpectrochimicaActa33B, 153 (1978)), propose to realize STLA approach way, be placed on pyrolysis coating graphite-pipe (PGT) with pyrolytic graphite platform (PGPF), at heating rate greater than 2000K/s, integration absorptiometry (Q
A).He is responsible for W.Slavin with AAS portion of PE company and formally begins to reach and cooperate decades (Slavin told the inventor in 1985, PE to L ' vov up to 1,000,000 dollars/year).Slavin carries out commercialization with L ' vov invention in PE company and is used for STLA analysis, promptly famous steady temperature platform graphite furnace technology (STPF) (W＞Slavinet.al; Anal.Chem.51,261 (1979), At.Spectrosc.2,137 (1981), GFAAS, A sourcebook, PE, Norwalk (1984), Spectrochimica Acta39B271 (1984)).The permanent magnetic field of Hitachi, Ltd production patent Earth Oxides by Zeeman GFAAS in 1977 (Z, PMGFAAS) 170-70 type, Varian in 1978 and PE the company alternating magnetic field of production patent simultaneously Earth Oxides by Zeeman GFAAS (Z, AMGFAAS) PEZ5000 type.The present inventor applied for from Chinese Academy of Sciences's cyclisation that 170,000 yuan were set up 19 people's development groups (bag is scraped 3 postgraduates), 170-70 instrument of import in 1977.Realize STLA approach way by L ' vov in 1976, carry out that comprehensively commodity HGA graphite furnace AAS is transformed into the instrument that can be used for STLA.(1) 1977 year and Shenyang metal institute cooperation research and development pyrolytic graphite production technology (happy year of horse, Zhang Wentao, Xu Guozhen, analytical chemistry 8 (5), 462 (1980)) fed nitrogen and propane flammable gas 5: 1 with carbon shirt-circuiting furnace, temperature 2000 degree, or induction furnace, ratio 2: 1,1850 degree.This technology free popularization in evaluation meeting given more than ten unit.PGT the earliest in a large amount of producing countries, PGPF, and full coating graphite tube (TPGT), Zao 2 years than PE company.Chinese Academy of Sciences's third prize and the adjustable graphite furnace power supply that is rapidly heated of Liaoning Province's second prize (2) (Zhang Zhongming, Li Shaoyuan, happy year of horse, environmental science 3 (6), 61 (1982)), than PE Zao 2 years.Get Chinese Academy of Sciences's third prize.(3) (the same, environmental science can accurately be measured temperature 400-3200K from printing 3 (2), 48 (1982) to thermo detector.(4) Rochon prism, the Sun Jian of cyclisation institute development.(5) permanent magnet, electricity section in Guilin develops.Succeeded in developing domestic first Z in (6) 1980 years, PMGFAAS, the ZM-1 type solves commodity HGA graphite furnace in the world first and is positioned over 10mm space, a magnet gap difficult problem (not applying for a patent), and body of heater thermal capacity is little, quick heating, argon gas consumes little, and the graphite-pipe life-span is long, in conjunction with using WTaPGT, TPGT, all 62 elements can measuring of successful analysis.Get Chinese Academy of Sciences's second prize.The 170-70 of Hitachi, 180-70, Z8000, Z8100, Z8200, and Z5000 type in 2000 fails to solve this difficult problem, body of heater thermal capacity is big, it is slow to heat up, and the power supply power consumption is big, can not measure 30 high temperature elements, the atomic absorption peak is short and wide, memory effect is serious, and argon gas consumption is big 3 liters/minute, and the graphite-pipe life-span is short.(5) patent No. is ZL96103243X, fixing patent No. G0IN21/31, fixed metal tungsten or tantalum platform-graphite tube and fixing means thereof, be called for short WTaPGT, invention in 1979, (Wu Zhengke, happy year of horse, China Environmental Science 4,65 (1981), chemistry circular 7,86 (1982), environmental chemistry 1 (3), 228 (1982)) must Chinese Academy of Sciences's third prize.(6) lining tungsten WTaPGT, patent " fixed metal tungsten or tantalum platform graphite tube preparation method (in application) " invention in 1984 (happy year of horse, Cheng Jianguo, analytical chemistry, 16 (3), 225 (1988), 18 (3), 266 (1990), spectroscopy and spectral analysis, 8 (2), 53 (1988)).(7) Z, PMGFAAS, the ZM-2 type comprises (2) adjustable power supply that is rapidly heated, (5) WTaPGT, the domestic and international steady temperature WTaPGT technology that did not up to the present have, integral measurement Q
A, (Jing Shilian, happy year of horse etc., spectroscopy and spectral analysis 5 (3), 62 (1985), Chinese Academy of Sciences's third prize.(8) ZM-1 and ZM-2 transfer the commodity Z the earliest in producing country in 1985 of Ministry of Nuclear Industry Suzhou 267 factories, PMGFAAS instrument WFX-Z type, Ministry of Nuclear Industry's second prize, produce three altogether, the unfortunate stopping production AAS in 1986 of 267 factories instrument.With ZM-2 and WFX-Z instrument, the best test feature amount m that steady temperature WTaPGT technology obtains
0Exp
*(62 elements) lists in table 1.
(9) among the fair-skinned discussion of the 1978-1980 Nian He postgraduate Feng ZGFAAS Zeeman splitting of ultimate analysis line to Zeeman absorptance (R
Z=ZGFAAS/GFAAS) influence (happy year of horse, Feng is fair-skinned, chemical journal, 40 (5), 425 pages and 439 pages, 42 (2), 137 (1984), spectroscopy and spectral analysis, 6 (2), 28 (1986)) with Zeeman analytic curve (ZQX).Chinese Academy of Sciences's third prize, Feng is fair-skinned to be chosen as one of best 20 postgraduates in 800 of this Chinese Academy of Sciences, horse happy year was one of best tutor.This work is in the leading level in the world, is engaged in Zao 8 years of ZQX research than L ' vov in 1986-1996.We draw the Zeeman splitting π and the σ composition figure of 180 analytical lines of 62 elements.Calculated overlap factor a=K in theory
σ/ K
z(Z, PMGFAAS), a=K
σ/ K
o(Z＜AMGFAAS) (c), A
O, σ=0.434K
σL, A
π, σ=0.434K
πL, A
σ, o=0.434K
oL (d), l are graphite-pipe length 28mm.A
σ, oBe the light absorption value A of Rochon prism at vertical light position and crooked ZQX linear zone (below 0.2)
⊥=A
σ=A
σ, 0, same A
π, 0Be light absorption value A in the directional light position
//=A
π=A
π, 0(below 0.2), A
σ, oLight absorption value A during for no Rochon prism
σ, o=A
o(below 0.2), the i.e. light absorption value of GFAAS.We derive theoretical Zeeman absorptance to Z, and PMGFAAS is R
Z, PM(1-a) K
π/ K
0(e), to Z, AMGFAAS is R
Z, AM=1-K
σ/ K
0(f), K
π/ K
0Be the division factor, the absorption that the division of expression π composition causes descends.We draw π and absorb line with Voigt function and formula of reduction, and σ absorbs the profile that line and normal (NAAS) absorb line, again according to the experimental formula Δ υ of Lorentz
s=0.36 Δ υ
LEmission line and absorption line profile are done relative displacement, use integration method again, can calculate the R of 62 elements theoretically
Z, PMValue.The experiment measured value ZM-1 of 62 elements, ZM-2, the WFX-Z instrument obtains, and theoretical and experiment value is consistent substantially.The same manner is asked R
Z, AMTheoretical value, experiment value are taken to PE Z5000 type instrument, and same theory conforms to substantially with experiment value.The R of 62 elements
Z, PM, R
Z, AMValue is listed in table 1.
Zeeman splitting (Zspl) shows with following formula matching graceful analytic curve (ZQX) influence, to Z, and PMGFAASA
Z=A
π-A
σ=-log (e
-K π l+ α)+log (e
-aK π l+ α) (g) α is a nonlinear factor, gets A with formula (d) substitution
Z=-log (10
-A π, 0+ α)+log (10
-ak π, 0+ α) (h) along with A
π, 0Increase (increase that is m among the ZQX (pg) amount), A
πAlso increase, reach platform gradually but influenced by α, and A at this moment
σStill be linear growth, subtract each other the result, A
ZBy rising to rollback point A
rValue just descends then.Therefore corresponding rollback point A in ZQX
rNonlinear factor will be α
*=(10
Ar-1)
-1(i) to Z, AMGFAAS has A
Z=A
0-A
σ=-log (10
-A σ, o+ α)+log (10
-aA π, o+ α) (j)
In order to estimate Zspl to the crooked influence of ZQX, 1982-1986 ZM-2, WFX-Z instrument, Q
AMeasure, steady temperature WTaPGT technology is studied 62 element ZQX, Mo, V, Ti, Ca, Sr, Ba, Os, Ir, Ru, Rh, TPGT graphite-pipe such as Pt, Pd etc.With the ZM-2 instrument of taking Rochon prism away, promptly the QX of single beam instrument compares.The QX that finds the non-Zeeman of bend ratio of ZQX wants serious, and this is because of the Δ υ at non-Zeeman
SplThe Δ υ of the new Zeeman splitting Zspl of last stack
ZsplFactor, Theoretical Calculation auxiliary view illness that has not attacked the vital organs of the human body is bright, and this influence is to reaching 0.4A
R, i.e. Q
AIn fact bending value can just begin bending up between the 1-1.5 more than 0.2, therefore crooked reason is not limited only to Δ υ
Hfs, Δ υ
ZsplTwo factors, other has new factor.Kh.Gilmutdinov et al, Spectrochimica Acta 46B, 1121 (1991), 47B, 1075 (1992), use similar camcorder technology to research and analyse element in graphite-pipe during atomization, atom distributes very inhomogeneous in graphite-pipe, thereby causes that curve is seriously crooked.Use xsect nonuniformity coefficient ρ and vertical two new coefficients of nonuniformity coefficient h, complete like this what ZAQX that resolves to, AQX is at Q
AGreater than just beginning bending more than 0.2.To solve α or α simultaneously in theory
*, Δ υ
Hfs, Δ υ
Zspl, ρ, the parameter influence of five coefficients of h, mathematic(al) mode is too complicated, is difficult to be extensive use of in the user, and this has become a new difficult point.Five coefficients must be simplified to two, just might solve with experiment and graph mode.B.V.L ' vov in 1996, Spectrochimica Acta 51B (6), 609 (1996), suggestion is Δ υ
Hfs, Δ υ
Z, spl, ρ, h, four coefficients are simplified to a unified tortuosity factor β, keep α or α
*Nonlinear factor proposes to use Q '
A, 0=Q
A, 0(1-β Q
A, 0) (k) substitution β=0, only consider α or α
*The time, by the Q that measures
ATry to achieve Q through linearization process
A, 0Formula (1), this formula present inventor just widely applies when 1978-1981 research ZAQX; Q
A=log (1+ α
*)/10
-(1+ α *) QA, 0+ α
*(1) at last consider β and α simultaneously
*(or α) is by the Q that measures
ATry to achieve Q through linearization process
A, 0Formula (m); Q
A=log (1+ α
*)/(10
-(1+ α *) QA, 0/ (1-β QA, 0)+ α
*) (m) directly formula (m) is used for Q
ATry to achieve Q through linearization
A, 0Computing is too complicated, therefore also with the experience of 1978-1980 research ZAQX, has only the tabulation experience of β=0 at that time, in table, and A
rValue is from 0.8-7.0 interval 0.1, Q
AFrom 0.1-0.9A
rInterval 0.1-0.2, this has been a huge form.The present inventor was retired in 1996, finished 18 big forms of different beta value alone; β is from-0.40, and-0.33 ,-0.27 ,-0.20 ,-0.14 ,-0.07,0 (having), 0.02,0.04,0.06,0.08,0.10,0.12,0.16,0.20,0.24,0.30,0.39.Having determined that the linearity between the different beta value is better, in tabulation, reduce length, at last 19 big forms are tapered to 7 big forms, promptly β is-0.40 ,-0.27 ,-0.14,0.00,0.10,0.24,0.39.Again the tabulation mode is changed into each A
rIt is a column that 7 β values are arranged in the value, Q
AFrom 0.1 to 0.9A
rInterval 0.1 to 0.2, A
rFrom 0.8-7.0 interval 0.1.All forms is listed in table 2.
There has been inventor after the table 2 to spend the several years work inventor since 1978 years to be worked and the data Q of domestic and foreign literature again
π-m (pg) AQX, ZAQX measures A up to ten thousand
r, the β value from atomization temperature T (K)=T ℃+200K, accesses m from table 1
0Cal, ε "=m
0Cal/m
0Exp
*, m
0Exp
*, measure Q
AM when the correspondence 0.0044 below 0.2
0Exp value, and correction coefficient k=m
0exp */ m
0The exp value.Verify up to ten thousand AQX, ZAQX shows, by the table 2 that formula (m) obtains, can be used for STLA fully with Q
ATry to achieve Q through linearization
A, 0AQX, the range of application of ZAQX can expand 0.9A to from original 0.2
r, enlarge tens of times.Concrete mensuration way will be discussed in four softwares of following A BCD.
(1) A software; Include 1:62 the m of element when different temperatures T (K)=T ℃+200K of table
0Cal, ε
A *=m
0Cal/m
0Exp
*, m
0Exp
*Value and Zeeman absorptance R
Z, PM and R
Z, the AM value.A software is divided into software three times by sequence of operation, by page turn over operation.(1) A1 software; Purpose is asked correction coefficient K=m
0Exp
*/ m
0Exp.Utilize among the table 3-6 volumetric solution 1 and No. 2, corresponding Q
A, 0=0.044 and 0.132, Q at this moment
A, 0=Q
AValue, K=m
0Exp
*Q
AR
Z＜PM/ 0.0044m (formula 1-4). the mean value of obtaining corresponding K (1) of 1 and No. 2 liquid and K (2) is the K value that records.(2) A2 software; Purpose is asked the inverse values A of Zeeman typical curve
r. with the Q of volumetric solution 5 or No. 6
AValue. (3) A3 software; Purpose is asked the tortuosity factor β of Zeeman typical curve. ask No. 3,4,5, volumetric solution of β. take a three-stage approach by the page turning order. and (a) A3,1 sub-software; Obtain 3,4 with formula 5,6, No. 5 corresponding Q of liquid
A, 0Value is 0.44,1.32, and 4.4. is with No. 5 liquid Q
A, 0(5) be example,
rTo Z, PMGFAAS, Q
A, 0(5)=0.0044Km (5) R
Z, PM/ m
0Exp
*(5) with to Z, AMGFAAS, Q
A, 0(5)=0.0044Km (5) R
Z, AM/ m
0Exp
*Obtain Q respectively with formula (5) or (6)
A, 0(3) and Q
A, 0(4).(b) A3,2 sub-softwares; Include table 2.Show each Q
AAt different A
rQ with the different beta correspondence
A, 0Value. (c) A3,3 sub-softwares; Use interpolation method, as shown in table 7, be example with No. 5 liquid, the Q that records
ADiffering is decided to be 0.1 or 0.2 round values, but at low Q
A(L) and contiguous high Q
A(H) between.The β that tries to achieve equally (5) must be between low β of two vicinities (L) and high β (H).
Table 7; Ask β with interpolation method
A
r β Q
A(L) Q
A(5) Q
A(H)
β(L) Q
A，0(L，β(L)) Q
A，0(5，β(L)) Q
A，0(H，β(L))
A
r(calibration value) β (5) Q
A, 0(5, β (5))=Q
A, 0(5)
B(H) Q
A，0(L，β(H)) Q
A，0(5，β(H)) Q
A，0(H，β(H))
As shown in table 7, available interpolation French (7) (8) (9).
Q
A，0(5，β(L))＝Q
A，0(L，β(L))+(Q
A(5)-Q
A(L))(Q
A，0(H，β(L))-Q
A，0(H，β(L))/(Q
A(H)-Q
A(L)) (7)
Q
A，0(5，β(H))＝Q
A，0(L，β(H))+(Q
A(5)-Q
A(L))(Q
A，0(H，β(H))-Q
A，0(L，β(H))/(Q
A(H)-Q
A(L)) (8)
β(5)＝β(L)+(β(H)-β(L))(Q
A，0(5，β(L))-Q
A，0(5))/Q
A，0(5，，β(L))-Q
A，0(5，β(H)) (9)
(2) B software; Obtain A with A software
r, β (Y) value is with the Q that measures
A(X) value is obtained Q through linearization
A, 0(X, β (Y)) value. use interpolation method,
Table 8; With interpolation method with Q
AValue is tried to achieve Q through linearization
A, 0Value
A
r β Q
A(L) Q
A(X) Q
A(H)
β(L) Q
A，0(L，β(L)) Q
A，0(X，β(L)) Q
A，0(H，β(L))
A
r(calibration value) β (Y) Q
A, 0(X, β (Y))
B(H) Q
A，0(L，β(H)) Q
A，0(X，β(H)) Q
A，0(H，β(H))
As shown in table 8, available interpolation French (10) (11) (12).
Q
A，0(X，β(L))＝Q
A，0(L，β(L))+(Q
A(X)-Q
A(L))(Q
A，0(H，β(L))-Q
A，0(L，β(L))/Q
A(H)-Q
A(L)) (10)
Q
A，0(X，β(H))＝Q
A，0(L，β(H))+(Q
A(X)-Q
A(L))(Q
A，0(X，β(H))-Q
A，0(L，β(H))/Q
A(H)-Q
A(L)) (11)
Get Q by formula (10) (11)
A, 0(X, β (Y))=Q
A, 0(X, β (L))+(β (Y)-β (L)) (Q
A, 0(X, β (H))-Q
A, 0(X, β (L))/β (H)-β (L)) (12).
(3) C software; Record constituent content m to be measured (pg) value with no standard analytical process fundamental formular 13,14. to Z, PMGFAAS instrument, m=Q
A, 0m
0Exp
*/ 0.0044KR
Z, PM(13), to Z, AMGFAAS instrument, m=Q
A, 0m
0Exp
*/ 0.0044KR
Z, AM(14)
(4) D software; With the m value that C software obtains, import fluid sample sampling volume V with formula 15
In(μ l), or with formula 16 input solid sample sample size mg.Obtain concentration C, liquid is pg/ μ l, and solid is the pg/mg value.C＝m/V
in(pg/μl，ng/ml，μg/l) (15)，C＝m/m
in(pg/mg，ng/g，μg/kg) (16)。
During with Zeeman deduction background GFAAS analytic sample, the serious bending of analytic curve causes and will analyze with a plurality of standard models, and this is to think for a long time to be difficult to realize no standard analysis one of the main reasons. and use this software will record Q
AValue is tried to achieve Q through linearization
A, 0, the available no standard analytical process fundamental formular of.Therefore this software is to realize the main and requisite core building block of no standard analysis.
Table 1 is 62 ms of element under different temperatures T (K) 3.
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
Table 1 is 62 ms of element under different temperatures T (K) 4.
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
Table 1 is 62 ms of element under different temperatures T (K) 5.
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
Table 1 is 62 ms of element under different temperatures T (K) 6.
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
Table 1 is 62 ms of element under different temperatures T (K) 7.
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
Table 1 is 62 ms of element under different temperatures T (K) 8.
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
Table 1 is 62 ms of element under different temperatures T (K) 9.
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
Table 1 is 62 ms of element under different temperatures T (K) 10.
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
(11) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
(12) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
(13) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
(14) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
(15) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
(16) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
(17) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
(18) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
(19) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value
(20) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A '=m
0Cal/m
0Exp
*, m
0Exp
*Value
(21) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A '=m
0Cal/m
0Exp
*, m
0Exp
*Value
(22) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A '=m
0Cal/m
0Exp
*, m
0Exp
*Value
(23) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A '=m
0Cal/m
0Exp
*, m
0Exp
*Value
(24) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A '=m
0Cal/m
0Exp
*, m
0Exp
*Value
(25) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A '=m
0Cal/m
0Exp
*, m
0Exp
*Value
(26) 62 ms of element under different temperatures T (K) of table 1
0Cal, ε
A '=m
0Cal/m
0Exp
*, m
0Exp
*Value
Table 2 3., from recording Q
AValue gets Q through linearization process
A, 0
Table 2 4., from recording Q
AValue gets Q through linearization process
A, 0
Table 2 5., from recording Q
AValue gets Q through linearization process
A, 0
Table 2 6., from recording Q
AValue gets Q through linearization process
A, 0
Table 3, the concentration of standard solution that permanent magnetic field Zeeman button background THGA graphite furnace uses
| Element | Li | Na | K | Rb | Cs | Cu | Ag | Au | Be | Mg | Ca | Sr |
| Wavelength (nm) | 670.8 | 589.0 | 766.5 | 780.0 | 852.1 | 324.7 | 328.1 | 2437 | 234.8 | 285.2 | 422.7 | 460.7 |
| Temperature (K) | 2400 | 1900 | 1800 | 1800 | 1900 | 2200 | 1900 | 2200 | 2500 | 2300 | 2600 | 2600 |
| m zexp *(pg) | 5.05 | 2.48 | 2.66 | 7.07 | 27.0 | 12.9 | 6.45 | 27.5 | 1.45 | 0.954 | 0.998 | 1.87 |
| Mark one (ng/ml) | 5.0 | 2.5 | 2.7 | 7.0 | 27.0 | 13.0 | 6.5 | 28 | 1.5 | 1.0 | 1.0 | 1.9 |
| Element | Ba | Zn | Cd | Hg | Al | Ga | In | Tl | Ge | Si | Sn | Pb |
| Wavelength (nm) | 553.5 | 213.9 | 228.8 | 253.7 | 309.2 | 287.4 | 303.9 | 276.7 | 265.2 | 251.6 | 286.3 | 283.3 |
| Temperature (K) | 260 | 1900 | 1600 | 1300 | 2500 | 2500 | 2200 | 1900 | 2600 | 2600 | 2400 | 1900 |
| m zexp *(pg) | 8.17 | 1.006 | 1.081 | 191 | 24.0 | 40.8 | 26.8 | 46.3 | 60.1 | 45.7 | 51.5 | 22.7 |
| Mark one (ng/ml) | 8.0 | 1.0 | 1.1 | 190 | 24.0 | 40 | 27 | 46 | 60 | 46 | 50 | 23 |
| Element | As | Sb | Bi | Bi | Se | Te | Cr | Cr | Mn | Fe | Co | Ni |
| Wavelength (nm) | 193.7 | 217.6 | 223.1 | 306.8 | 196.0 | 214.3 | 357.9 | 359.3 | 279.5 | 248.3 | 240.7 | 232.0 |
| Temperature (K) | 2400 | 2400 | 2000 | 2000 | 2200 | 2200 | 2500 | 2500 | 2300 | 2500 | 2500 | 2600 |
| m zexp *(pg) | 39.6 | 56.5 | 58.9 | 347 | 51.2 | 68.8 | 8.66 | 6.25 | 7.57 | 11.4 | 11.3 | 17.9 |
| Mark one (ng/ml) | 40 | 27 | 60 | 35 | 51 | 70 | 9.0 | 6.0 | 7.6 | 11.0 | 11.0 | 18.0 |
| Element | Pd | Pt | Rh | Ru | Sc | Y | Eu | Dy | Ho | Er | Tm | Yb |
| Wavelength (nm) | 247.6 | 265.9 | 343.5 | 349.9 | 391.2 | 410.2 | 459.4 | 421.2 | 410.4 | 400.8 | 371.8 | 398.8 |
| Temperature (K) | 2500 | 2600 | 2600 | 2600 | 2700 | 2700 | 2600 | 2700 | 2700 | 2700 | 2600 | 2500 |
| m zexp *(pg) | 35.8 | 180 | 40.0 | 90.0 | 20.3 | 121 | 24.3 | 49.4 | 39.9 | 43.3 | 9.4 | 3.06 |
| Mark one (ng/ml) | 36 | 180 | 40 | 90 | 20 | 120 | 24 | 50 | 40 | 43 | 9.0 | 3.0 |
| Element | P | Os | B | La | Ce | Pr | Nd | Sm | Gd | Tb | Lu | U |
| Wavelength (nm) | 213.6 | 290.9 | 249.8 | 550.1 | 463.2 | 495.1 | 463.4 | 429.7 | 407.9 | 432.6 | 336.0 | 358.5 |
| Temperature (K) | 2600 | 3100 | 2700 | 2700 | 2700 | 2700 | 2700 | 2700 | 2700 | 2700 | 2700 | 2700 |
| m zexp *(ng) | 12.3 | 1.82 | 0.333 | 1.61 | 42.3 | 1.83 | 0.963 | 0.335 | 3.23 | 0.370 | 0.568 | 5.51 |
| Mark one (μ g/ml) | 12.0 | 1.8 | 0.33 | 1.6 | 42 | 1.8 | 1.0 | 0.33 | 3.2 | 0.37 | 0.57 | 5.5 |
| Element | Ir | Ti | V | Mo | ||||||||
| Wavelength (nm) | 265.0 | 365.4 | 318.5 | 313.3 | ||||||||
| Temperature (K) | 2600 | 2700 | 2700 | 2700 | ||||||||
| m zexp *(pg) | 141 | 70.0 | 52.3 | 28.6 | ||||||||
| Mark one (ng/ml) | 140 | 70 | 52 | 30 |
Table 4, the volumetric solution concentration ng/ml that permanent magnetic field Zeeman button background HGA graphite furnace uses
Table 5, the volumetric solution concentration ng/ml that alternating magnetic field Zeeman button background HGA graphite furnace uses
Table 6, the volumetric solution concentration ng/ml that alternating magnetic field Zeeman button background THGA graphite furnace uses
Claims (2)
1; No standard analysis comprises with software in the Zeeman button back of the body graphite furnace atomic absorption photometer of the present invention;
(1) A software; Include table 1; 62 ms of element when different temperatures T (K)=T ℃+200K
0Cal, ε
A'=m
0Cal/m
0Exp
*, m
0Exp
*Value and Zeeman absorptance R
Z, PM and R
Z, the AM value.A software is divided into software three times by sequence of operation, by page turn over operation.(1) A1 time than part; Purpose is asked correction coefficient K=m
0Exp
*/ m
0Exp.Utilize among the table 3-6 volumetric solution 1 and No. 2, corresponding Q
A, 0=0.044 and 0.132, Q at this moment
A, 0=Q
AValue, K=m
0Exp
*Q
AR
Z＜PM/ 0.0044m (formula 1-4). the mean value of obtaining corresponding K (1) of 1 and No. 2 liquid and K (2) is the K value that records.(2) A2 software; Purpose is asked the inverse values A of Zeeman typical curve
rQ with volumetric solution 5 or No. 6
AValue. (3) A3 software; Purpose is asked the tortuosity factor β of Zeeman typical curve.Ask No. 3,4,5, volumetric solution of β.Take a three-stage approach by the page turning order.(a) A3,1 sub-software; Obtain 3,4 with formula 5,6, No. 5 corresponding Q of liquid
A, 0Value is 0.44,1.32,4.4.With No. 5 liquid Q
A, 0(5) be example, to Z, PMGFAAS, Q
A, 0(5)=0.0044Km (5) R
Z, PM/ m
0Exp
*(5) with to Z, AMGFAAS, Q
A, 0(5)=0.0044Km (5) R
Z, AM/ m
0Exp
*(6), obtain Q respectively with formula (5) or (6)
A, 0(3) and Q
A, 0(4).(b) A3,2 sub-softwares; Include table 2.Show each Q
AAt different A
rQ with the different beta correspondence
A, 0Value.(c) A3,3 sub-softwares; Use interpolation method, as shown in table 7, be example with No. 5 liquid, the Q that records
ADiffering is decided to be 0.1 or 0.2 round values, but at low Q
A(L) and contiguous high Q
A(H) between.The β that tries to achieve equally (5) must be between low β of two vicinities (L) and high β (H). and 7-9 can obtain the β value with the interpolation French.Q
A，0(5，β(L))＝Q
A，0(L，β(L))+(Q
A(5)-Q
A(L))(Q
A，0(H，β(L))-Q
A，0(H，β(L))/(Q
A(H)-Q
A(L)) (7)Q
A，0(5，β(H))＝Q
A，0(L，β(H))+(Q
A(5)-Q
A(L))(Q
A，0(H，β(H))-Q
A，0(L，β(H))/(Q
A(H)-Q
A(L)) (8)β(5)＝β(L)+(β(H)-β(L))(Q
A，0(5，β(L))-Q
A，0(5))/(Q
A，0(5，，β(L))-Q
A，0(5，β(H)) (9)
(2) B software; Obtain A with A software
r, β (Y) value is with the Q that measures
A(X) value is obtained Q through linearization
A, 0(X, β (Y)) value.Use interpolation method, as shown in table 8, Q
A, 0(X, β (L))=Q
A, 0(L, β (L))+(Q
A(X)-Q
A(L)) (Q
A, 0(H, β (L))-Q
A, 0(L, β (L))/Q
A(H)-Q
A(L)) (10) Q
A, 0(X, β (H))=Q
A, 0(L, β (H))+(Q
A(X)-Q
A(L)) (Q
A, 0(X, β (H))-Q
A, 0(L, β (H))/(Q
A(H)-Q
A(L)) (11) get Q by formula (10) (11)
A, 0(X, β (Y))=Q
A, 0(X, β (L))+(β (Y)-β (L)) (Q
A, 0(X, β (H))-Q
A, 0(X, β (L))/β (H)-β (L)) (12).
(3) C software: record constituent content m to be measured (pg) value with no standard analytical process fundamental formular 13,14.To Z, PMGFAAS instrument, m=Q
A, 0m
0Exp
*/ 0.0044KR
Z, PM(13), to Z, AMGFAAS instrument, m=Q
A, 0m
0Exp
*/ 0.0044KR
Z, AM(14)
(4) D software; With the m value that C software obtains, import fluid sample sampling volume V with formula 15
In(μ l), or with formula 16 input solid sample sample size mg.Obtain concentration C, liquid is pg/ μ l, and solid is the pg/mg value.C＝m/V
in(pg/μl，ng/ml，μg/l) (15)，C＝m/m
in(pg/mg，ng/g，μg/kg) (16)。
2, described according to claim 1;
During with Zeeman deduction background GFAAS analytic sample, the serious bending of analytic curve causes and will analyze with a plurality of standard models, and this is to think for a long time to be difficult to realize no standard analysis one of the main reasons.Use this software will record Q
AValue is tried to achieve Q through linearization
A, 0, the available no standard analytical process fundamental formular of.Therefore this software is to realize the main and requisite core building block of no standard analysis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100937733A CN101319992A (en) | 2008-04-21 | 2008-04-21 | Software for non-standard analysis of Zeeman background graphite furnace atomic absorption photometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100937733A CN101319992A (en) | 2008-04-21 | 2008-04-21 | Software for non-standard analysis of Zeeman background graphite furnace atomic absorption photometer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101319992A true CN101319992A (en) | 2008-12-10 |
Family
ID=40180164
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008100937733A Pending CN101319992A (en) | 2008-04-21 | 2008-04-21 | Software for non-standard analysis of Zeeman background graphite furnace atomic absorption photometer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101319992A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101692040B (en) * | 2009-04-02 | 2012-07-04 | 马怡载 | Multi-element measurement atomic fluorescence photometer of continuous light source of energy-saving low-price tungsten wire ring furnace |
| CN101692041B (en) * | 2009-04-02 | 2013-01-23 | 马怡载 | Tungsten or tantalum platform-graphite tube atomic absorption photometer for measuring multiple elements |
| CN101692039B (en) * | 2009-04-02 | 2013-03-27 | 马怡载 | Energy-efficient and low-cost tungsten wire coil furnace atomic absorption photometer for measuring multiple elements forming hollow cathode lamp |
-
2008
- 2008-04-21 CN CNA2008100937733A patent/CN101319992A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101692040B (en) * | 2009-04-02 | 2012-07-04 | 马怡载 | Multi-element measurement atomic fluorescence photometer of continuous light source of energy-saving low-price tungsten wire ring furnace |
| CN101692041B (en) * | 2009-04-02 | 2013-01-23 | 马怡载 | Tungsten or tantalum platform-graphite tube atomic absorption photometer for measuring multiple elements |
| CN101692039B (en) * | 2009-04-02 | 2013-03-27 | 马怡载 | Energy-efficient and low-cost tungsten wire coil furnace atomic absorption photometer for measuring multiple elements forming hollow cathode lamp |
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