CN104897634A - Internal standard method for testing element prone to chemical vapor generation reaction through atomic fluorescence - Google Patents
Internal standard method for testing element prone to chemical vapor generation reaction through atomic fluorescence Download PDFInfo
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Abstract
The invention provides an internal standard method for testing an element prone to a chemical vapor generation reaction through atomic fluorescence and belongs to the technical field of instrument assay determination. The internal standard method comprises steps as follows: a to-be-tested element excitation light source is selected, a blank intensity value of the to-be-tested element is acquired and taken as an internal standard element intensity value, and an atomic fluorescence intensity value of the to-be-tested element is acquired; a standard solution containing the to-be-tested element is selected, the specific value of the atomic fluorescence intensity value of the to-be-tested element in the standard solution to an atomic fluorescence intensity value of an internal standard element is tested, and a standard calibration curve about the concentration of the standard solution of the to-be-tested element is built. An improved method is put forward based on influence factors such as acidity of a sample solution during a generation reaction, interference of coexisting elements in the sample solution, fluctuation of the conveying process of formed vapor entering an atomizer, fluctuation of an atomic fluorescence lighting source, environmental temperature changes and the like when a sample introduced through chemical vapor generation is tested through a non-dispersive atomic fluorescence spectrophotometer, and accordingly, the correlation of the standard calibration curve as well as the precision and the accuracy of a test result are improved during testing.
Description
Technical field
The invention belongs to instrumental analysis determination techniques field, particularly relate to the easy chemical evapn of a kind of atom fluorimetry react element time internal standard method.
Background technology
Chemical evapn is a kind of sampling technique separated from sample solution based on the gaseous compound utilizing chemical reaction to make element to be measured form volatilization, be improve sensitivity of analytical method and optionally effective way, be widely used in atomic spectroscopic analysis at present.These utilize chemical evapn react sample introduction measure unit have antimony, bismuth, mercury, selenium, tellurium, lead, germanium, lead, zinc, tin, gold, chromium, cadmium, silver.But when using hydride-atomic fluorescence of zero dispersion to measure above-mentioned element, but finding that there is several factors and affecting measurement result greatly.These factors comprise: when reacting in the acidity of sample solution, sample solution coexistence elements interference, form steam after enter the temperature drift, variation of ambient temperature etc. of the fluctuation of atomizer transmitting procedure, the fluctuation of atomic fluorescence excitation source and drift, atomizer.Experiment proves: the existence of above-mentioned factor, standards calibration curve correlativity can be made to degenerate, make precision of measurement variation, make the error amount of measurement accuracy of measurement become large.
Therefore need badly in the middle of prior art and want a kind of novel technical scheme to solve this problem.
Summary of the invention
Technical matters to be solved by this invention is: provide the easy chemical evapn of a kind of atom fluorimetry react element time internal standard method, for chemical evapn generation sample introduction, also exist during atomic fluorescence of zero dispersion photometric determination react time sample solution acidity, the interference of coexistence elements in sample solution, the fluctuation of atomizer transmitting procedure is entered after forming steam, the fluctuation of atomic fluorescence excitation source and drift, the temperature drift of atomizer, the influence factors such as variation of ambient temperature, the method improved is proposed, thus improve the correlativity surveying timing standard calibration curve, the preci-sion and accuracy of measurement result.
The easy chemical evapn of atom fluorimetry react element time an internal standard method, it is characterized in that: comprise the following steps,
Step one, choose element excitation source to be measured, adopt pulse lighting mode, sequential illumination atomizer in chronological sequence, the blank intensity level obtaining element to be measured, as internal standard element intensity level, is designated as I
interior mark, obtain the atomic fluorescence intensity level of element to be measured, be designated as I
analyze;
Wherein, element to be measured is that the instrument parameter of arsenic element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 300ml/min, shield gas flow amount 800ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of antimony element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 300ml/min, shield gas flow amount 800ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of bismuth element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of mercury element is as follows: negative high voltage 270V ~ 300V, lamp current 15mA ~ 40mA, atomizer height 10mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of selenium element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of tellurium element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of tin element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of lead element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of cadmium element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of Zn-ef ficiency is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 600ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of Ge element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 600ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Step 2, to choose containing concentration of element scope to be measured at the solution of 0.01 μ g/ml ~ 5.0 μ g/ml as standard solution, in bioassay standard solution, the ratio of the atomic fluorescence intensity level of element to be measured and the atomic fluorescence intensity level of internal standard element, is designated as I
analyze/ I
interior mark, with I
analyze/ I
interior markvalue to the concentration Criterion calibration curve of elemental standards solution to be measured;
Step 3, maintenance step one Instrumental parameter constant, choose sample for determining component content to be measured, measure the intensity level ratio of tested element and internal standard element in sample, be designated as I
sample/ I
interior mark, from the standards calibration curve that described step 2 is set up, obtain tested constituent content in sample.
In described step one, element to be measured comprises arsenic, antimony, bismuth, mercury, selenium, tellurium, lead, germanium, lead, zinc, tin, gold, chromium, cadmium, silver.
By above-mentioned design proposal, the present invention can bring following beneficial effect: the easy chemical evapn of a kind of atom fluorimetry react element time internal standard method, for chemical evapn generation sample introduction, also exist during atomic fluorescence of zero dispersion photometric determination react time sample solution acidity, the interference of coexistence elements in sample solution, the fluctuation of atomizer transmitting procedure is entered after forming steam, the fluctuation of atomic fluorescence excitation source and drift, the temperature drift of atomizer, the influence factors such as variation of ambient temperature, the method improved is proposed, thus improve the correlativity surveying timing standard calibration curve, the preci-sion and accuracy of measurement result.This method effectively can eliminate the interference of various factors, improves the correlativity of standards calibration curve; This method effectively can eliminate the transmission disturbance after steam generation, instrument drift, and then improves the preci-sion and accuracy of measurement result; This method can effectively eliminate chemical evapn react exist Physical Interference and chemistry disruption.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated:
Fig. 1 be the easy chemical evapn of a kind of atom fluorimetry of the present invention react element time internal standard method sample size measure process schematic.
Embodiment
The easy chemical evapn of atom fluorimetry react element time an internal standard method, as shown in Figure 1, comprise the following steps,
Step one, choose element excitation source to be measured, adopt pulse lighting mode, sequential illumination atomizer in chronological sequence, the blank intensity level obtaining element to be measured, as internal standard element intensity level, is designated as I
interior mark, obtain the atomic fluorescence intensity level of element to be measured, be designated as I
analyze; Its instrument parameter sees table:
The key instrument conditional parameter of table 1 arsenic element
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 300ml/min |
| Lamp current | 60-80mA | Shield gas flow amount | 800ml/min |
| Atomizer height | 8mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The key instrument conditional parameter of table 2 antimony element
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 300ml/min |
| Lamp current | 60-80mA | Shield gas flow amount | 800ml/min |
| Atomizer height | 8mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The key instrument conditional parameter of table 3 bismuth element
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 400ml/min |
| Lamp current | 60-80mA | Shield gas flow amount | 1000ml/min |
| Atomizer height | 8mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The key instrument conditional parameter of table 4 mercury element
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 400ml/min |
| Lamp current | 15-40mA | Shield gas flow amount | 1000ml/min |
| Atomizer height | 10mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The key instrument conditional parameter of table 5 selenium element
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 400ml/min |
| Lamp current | 60-80mA | Shield gas flow amount | 1000ml/min |
| Atomizer height | 8mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The key instrument conditional parameter of table 6 tellurium element
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 400ml/min |
| Lamp current | 60-80mA | Shield gas flow amount | 1000ml/min |
| Atomizer height | 8mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The key instrument conditional parameter of table 7 tin element
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 400ml/min |
| Lamp current | 60-80mA | Shield gas flow amount | 1000ml/min |
| Atomizer height | 8mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The key instrument conditional parameter of table 8 lead element
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 400ml/min |
| Lamp current | 60-80mA | Shield gas flow amount | 1000ml/min |
| Atomizer height | 8mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The key instrument conditional parameter of table 9 cadmium element
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 400ml/min |
| Lamp current | 60-80mA | Shield gas flow amount | 1000ml/min |
| Atomizer height | 8mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The key instrument conditional parameter of table 10 Zn-ef ficiency
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 600ml/min |
| Lamp current | 60-80mA | Shield gas flow amount | 1000ml/min |
| Atomizer height | 8mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The key instrument conditional parameter of table 11 Ge element
| Instrument condition | Parameter | Instrument condition | Parameter |
| Negative high voltage | 270-300V | Carrier gas flux | 600ml/min |
| Lamp current | 60-80mA | Shield gas flow amount | 1000ml/min |
| Atomizer height | 8mm | Reading duration | 10.0s |
| Atomizer temperature | 200℃ | Time delay | 1.0s |
The instrument condition parameter of each element above, can change to some extent along with the factor such as kind, the instrument of different manufacturers, the environment of test of institute's test sample product, and the change of above-mentioned instrument parameter numeral or extension are all in claims.
Step 2, to choose containing concentration of element scope to be measured at the solution of 0.01 μ g/ml ~ 5.0 μ g/ml as standard solution, in bioassay standard solution, the ratio of the atomic fluorescence intensity level of element to be measured and the atomic fluorescence intensity level of internal standard element, is designated as I
analyze/ I
interior mark, with I
analyze/ I
interior markvalue to the concentration Criterion calibration curve of elemental standards solution to be measured;
Step 3, maintenance step one Instrumental parameter constant, choose sample for determining component content to be measured, measure the intensity level ratio of tested element and internal standard element in sample, be designated as I
sample/ I
interior mark, from the standards calibration curve that described step 2 is set up, obtain tested constituent content in sample.
Embodiment 1,
Use arsenic high-strength hollow cathode fluorescent lamp, adopt pulse mode to light, successively take the blank atomic fluorescence signal of arsenic and the atomic fluorescence signal of arsenic mark liquid or sample in chronological order; The hydrochloric acid solution 10ml of 1:1 is added in the volumetric flask of one group of 50.0ml, pipette the arsenic standard solution of the 1.0 μ g/ml of 0.00ml, 0.50ml, 1.00ml, 1.50ml, 2.00ml, 4.00ml in above-mentioned serial volumetric flask, add 10ml5% thiocarbamide and 5% ascorbic acid solution, rare to scale with water, shake up; The mensuration of carrying out arsenic is described according to atom fluorimetry, after mensuration, the arsenic element blank value recorded and fluorescent value is carried out strength ratio calculating as stated above, drawing standard calibration curve; Clear up one group of sample GBW07401, GBW07402, GBW07403 according to the digestion procedure of geological sample in DZG93-01, by identical conditions test, use internal standard method and do not use internal standard method, result is as following table 12,13.
The contrast of indices when table 12 internal standard method and conventional method survey arsenic
| Method | Calibration curve correlativity | Precision (RSD%) | Detection limit (μ g/g) |
| Conventional method | 0.9976 | 2.86 | 0.085 |
| Internal standard method | 0.9994 | 0.83 | 0.009 |
The contrast of accuracy when table 13 internal standard method and conventional method survey arsenic
Find out from table 12,13, after using this internal standard method, the correlativity of typical curve and detection limit, the preci-sion and accuracy of sample has had great improvement.
Embodiment 2,
Use mercury high-strength hollow cathode fluorescent lamp, adopt pulse mode to light, successively take the blank atomic fluorescence signal of mercury and the atomic fluorescence signal of mercury mark liquid or sample in chronological order; The potassium bichromate solution of the salpeter solution 10ml and 5% of 1:1 is added in the volumetric flask of one group of 50.0ml, pipette the mercury standard solution of the 0.010 μ g/ml of 0.00ml, 0.25ml, 0.50ml, 1.00ml, 2.00ml, 4.00ml in above-mentioned serial volumetric flask, rare to scale with water, shake up; The mensuration of carrying out mercury is described according to atom fluorimetry, after mensuration, the arsenic element blank value recorded and fluorescent value is carried out strength ratio calculating as stated above, drawing standard calibration curve; Clear up one group of sample GBW07301a, GBW07302a, GBW07303a according to the digestion procedure of geological sample in DZG93-01, by identical conditions test, use internal standard method and do not use internal standard method, result is as following table 14,15.
The contrast of indices when table 14 internal standard method and conventional method survey mercury
| Method | Calibration curve correlativity | Precision (RSD%) | Detection limit (μ g/g) |
| Conventional method | 0.9974 | 3.52 | 0.0076 |
| Internal standard method | 0.9993 | 0.63 | 0.0008 |
The contrast of accuracy when table 15 internal standard method and conventional method survey mercury
Find out from table 14,15, after using this internal standard method, the correlativity of typical curve and detection limit, the preci-sion and accuracy of sample has had great improvement.
Claims (2)
1. the easy chemical evapn of atom fluorimetry react element time an internal standard method, it is characterized in that: comprise the following steps,
Step one, choose element excitation source to be measured, adopt pulse lighting mode, sequential illumination atomizer in chronological sequence, the blank intensity level obtaining element to be measured, as internal standard element intensity level, is designated as I
interior mark, obtain the atomic fluorescence intensity level of element to be measured, be designated as I
analyze;
Wherein, element to be measured is that the instrument parameter of arsenic element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 300ml/min, shield gas flow amount 800ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of antimony element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 300ml/min, shield gas flow amount 800ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of bismuth element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of mercury element is as follows: negative high voltage 270V ~ 300V, lamp current 15mA ~ 40mA, atomizer height 10mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of selenium element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of tellurium element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of tin element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of lead element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of cadmium element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 400ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of Zn-ef ficiency is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 600ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Element to be measured is that the instrument parameter of Ge element is as follows: negative high voltage 270V ~ 300V, lamp current 60mA ~ 80mA, atomizer height 8mm, atomizer temperature 200 DEG C, carrier gas flux 600ml/min, shield gas flow amount 1000ml/min, reading duration 10.0s, time delay 1.0s;
Step 2, to choose containing concentration of element scope to be measured at the solution of 0.01 μ g/ml ~ 5.0 μ g/ml as standard solution, in bioassay standard solution, the ratio of the atomic fluorescence intensity level of element to be measured and the atomic fluorescence intensity level of internal standard element, is designated as I
analyze/ I
interior mark, with I
analyze/ I
interior markvalue to the concentration Criterion calibration curve of elemental standards solution to be measured;
Step 3, maintenance step one Instrumental parameter constant, choose sample for determining component content to be measured, measure the intensity level ratio of tested element and internal standard element in sample, be designated as I
sample/ I
interior mark, from the standards calibration curve that described step 2 is set up, obtain tested constituent content in sample.
2. the easy chemical evapn of a kind of atom fluorimetry according to claim 1 react element time internal standard method, it is characterized in that: in described step one, element to be measured comprises arsenic, antimony, bismuth, mercury, selenium, tellurium, lead, germanium, lead, zinc, tin, gold, chromium, cadmium, silver.
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