CN109406429A - A method of the atomic absorption spectroscopy determination content of heavy metal lead without matrix modifier - Google Patents
A method of the atomic absorption spectroscopy determination content of heavy metal lead without matrix modifier Download PDFInfo
- Publication number
- CN109406429A CN109406429A CN201811493888.1A CN201811493888A CN109406429A CN 109406429 A CN109406429 A CN 109406429A CN 201811493888 A CN201811493888 A CN 201811493888A CN 109406429 A CN109406429 A CN 109406429A
- Authority
- CN
- China
- Prior art keywords
- lead
- solution
- sample
- nitric acid
- atomic absorption
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a kind of methods of the atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier, react to form plumbi nitras with the lead ion in sample using dust technology, it heats up in graphite furnace by continuous discontinuity, moist plumbi nitras, which starts to decompose when 100 DEG C, is initially formed basic lead nitrate, continue heating and is then converted into lead oxide, lead oxide (strict control inert gas tail is blown) under the auxiliary of inert gas is interrupted by a narrow high temperature in a very short period of time, lead oxide is set to become elementary lead then by atomization, to calculate the lead content in sample by the special spectrum after measurement atomization, it can reduce testing cost (no matrix modifier), can effectively evade it is linear it is unstable caused by error, accuracy high-precision is good and has wider linear test scope, fully meet various contain Measure the measurement of lead.
Description
Technical field
The invention belongs to analyze testing field, and in particular to a kind of atomic absorption spectrophotometry survey of no matrix modifier
Determine the method for content of heavy metal lead.
Background technique
Heavy metal lead element is widely present in nature, and there are three aspects for the lead main source in organic matter: first is that work
The industry three wastes (exhaust gas, waste water, waste) pollute crops；Second is that lead in plant mainly adsorbs atmosphere, water, the knot of lead in soil
Fruit, the root of plant are not easy to absorb lead, and mainly leaf absorbs lead from air.Leaded pesticide, food additives or processing aid
Use；Third is that lead dissolves out in organic matter packing container and packaging material, caused by pollution.
Lead is mainly manifested in the following aspects to the harm of human body, neurological symptom: headache, has a sleepless night, is dizzy at agitation
It is dizzy.Gastrointestinal symptom: abdominal pain, Nausea and vomiting.Reproductive system: inhibition becomes pregnant, increases miscarriage, premature labor, premature rupture of fetal membranes, stillborn foetus
Possibility.Children are endangered: knowing the influence of energy, mental behavior growth.
Existing frequently-used detection method is that the way of matrix modifier is added to leaded sample to realize effective detection
Method, common matrix modifier are as follows: the substances such as palladium nitrate, ammonium di-hydrogen phosphate, nitric acid beauty.When in certain matrix modifiers
Metallics and sample in lead formed alloy after, when passing through atomic excitation, the excitation temperature needed is excessively high, and appearance cannot be complete
It is excited or is excited non-uniform phenomenon entirely, a double end peak is obtained so as to cause test structure and deviates truthful data.
In view of the foregoing, the method for needing to invent lead content in a kind of specific determination organic matter, there is its test method
Effect and simplicity.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of atomic absorption spectroscopy determinations of no matrix modifier
The method of content of heavy metal lead.
For achieving the above object, the invention provides the following technical scheme:
1, a kind of method of the atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier, the method
For atomic absorption spectrophotometry, matrix modifier is not used in the method.
Preferably, described method includes following steps:
(1) it prepares solution: preparing the nitric acid solution and 1mol/L of 0.5mol/L with the nitric acid of excellent pure grade and deionized water
Nitric acid solution；Matched with the nitric acid of excellent pure grade and the perchloric acid of excellent pure grade according to the volume mixture of 9:1 and mixed acid solution is made；
(2) prepare the lead standard solution of 100ng/mL: using the 0.5mol/L in step (1) nitric acid solution and go from
Sub- water is prepared；
(3) sample solution and blank reagent are prepared using wet resolution method or dry resolution method: utilizes the mixing in step (1)
The nitric acid solution of acid solution and 0.5mol/L prepare sample solution, using process preparation blank examination same as sample solution is prepared
Agent；
(4) it utilizes the light absorption value of the lead standard solution of atomic absorption spectroscopy determination 100ng/mL: using step (1)
The nitric acid solution of middle 0.5mol/L configures the lead standard solution to form different lead contents from the lead standard solution of 100ng/mL,
With the light absorption value of the lead standard solution of atomic absorption spectroscopy determination difference lead content, then with lead in lead standard solution
Ion concentration is abscissa, corresponding light absorption value is that ordinate obtains unary linear regression equation；
(5) light absorption value of blank reagent and the light absorption value of sample solution are measured respectively using atomic absorption spectrophotometry,
It substitutes into step (4) and obtains the lead content of blank reagent and the lead content of sample solution in unary linear regression equation；
(6) lead content in every gram of sample of sample is calculated.
Further, mark method, the heating procedure of the graphite furnace are matched using graphite furnace in the atomic absorption spectrophotometry
It is as follows:
A. it is warming up to 60 DEG C within the time of 3s, while argon gas is passed through with the speed of 0.10L/min；B. in the time of 20s
120 DEG C are inside warming up to, while argon gas is passed through with the speed of 0.10L/min；C. it is warming up to 250 DEG C within the time of 10s, while with
The speed of 0.10L/min is passed through argon gas；D. it is warming up to 450 DEG C within the time of 5s and keeps the temperature 10s, while with 1.00L/min's
Speed is passed through argon gas；E. 3s is kept the temperature at 450 DEG C in the case where obstructed argon gas；F. 1800 DEG C are warming up within the time of 5s；
G. it is warming up to 2500 DEG C within the time of 2s, while argon gas is passed through with the speed of 1.00L/min.
Further, the preparation method of lead standard solution described in step (2) specifically: absorption product type is GBW (E)
In 080129 lead single element standard substance 1.0mL to 100mL volumetric flask, the nitric acid solution of the 0.5mol/L is added to scale
The lead standard solution of 1.0 μ g/mL is obtained, then is drawn in lead standard solution 10mL to the 100mL volumetric flask of 1.0 μ g/mL, is added
Nitric acid solution to the scale for entering the 0.5mol/L obtains 100ng/mL lead standard solution.
Further, wet resolution method described in step (3) prepares the specific steps of sample solution are as follows: weighs sample 1.0000g
In conical flask, it is put into bead, the mixed acid solution soaked overnight of 15mL is added, it is straight in carrying out cutting down on electric furnace or heating plate
Become micro- yellow or transparent to solution, resolution catches up with acid to white cigarette to disperse；The hydrogen peroxide for being added 30% continues abatement to dry, addition
Scale is settled to after the nitric acid solution of 0.5mol/L into volumetric flask and with deionized water.
Further, the specific steps that resolution method prepares sample solution are done described in step (3) are as follows: weigh sample 1.0000g
In porcelain crucible, first small fire is carbonized in adjustable electric hot plate until do not smolder, move into ashing 6 at 475~525 DEG C of Muffle furnace~
It is cooling after 8h；The nitric acid solution that 0.5mol/L is added moves back ash content dissolution in volumetric flask, is repeatedly washed on a small quantity with deionized water
Porcelain crucible is washed, washing lotion is merged into volumetric flask, then is settled to scale with deionized water.
Further, the test process of lead standard solution light absorption value described in step (4) are as follows: take described in step (2)
The lead standard solution of 100ng/mL and the nitric acid solution of 0.5mol/L execute graphite furnace with mark in graphite furnace automatically nearly sample device
Method, each point
Sample introduction composition is respectively as follows: the nitric acid solution of the 0.5mol/L of+20 μ L of the lead standard solution of 0 μ L, 2 μ L
The nitric acid solution of the 0.5mol/L of+18 μ L of the lead standard solution, 4 μ L+16 μ L of the lead standard solution
The nitric acid solution of the 0.5mol/L, the nitric acid solution of the 0.5mol/L of+12 μ L of the lead standard solution of 8 μ L, 12 μ
The nitric acid solution of the 0.5mol/L of+8 μ L of the lead standard solution of L ,+4 μ L of the lead standard solution of 16 μ L
The nitric acid solution of the 0.5mol/L measures the light absorption value of each point with atomic absorption spectrophotometry.
Further, the test process of blank reagent light absorption value described in step (5) are as follows: draw 20 μ L of blank reagent, injection
Graphite furnace measures its light absorption value with atomic absorption spectrophotometry.
Further, the test process of the light absorption value of sample solution described in step (5) are as follows: 20 μ L of pipette samples solution, note
Enter graphite furnace, measures its light absorption value with atomic absorption spectrophotometry.
Further, the formula used in calculating described in step (6) are as follows: lead tolerance=(sample solution in every gram of sample
Lead content-blank reagent lead content)/sample quality.
The beneficial effects of the present invention are: the invention discloses a kind of atomic absorption spectrophotometries of no matrix modifier
The method for measuring content of heavy metal lead, i.e., react to form plumbi nitras using dust technology in lead, between passing through continuously in graphite furnace
Disconnected property heating, moist plumbi nitras start to decompose when 100 DEG C, are initially formed basic lead nitrate, continue heating and are then converted into oxidation
Lead, lead oxide (strict control inert gas tail is blown) under the auxiliary of inert gas are narrow by one in a very short period of time
High temperature interruption makes lead oxide become elementary lead then by atomization, to be calculated by the special spectrum after measurement atomization
Lead content in sample.Measuring method of the invention has the advantage that
(1) realizing equally can be with Accurate Determining lead content without matrix modifier for disturbed specimen, and inspection cost is significantly
It reduces；
(2) good linearity of measuring method, effectively evaded it is linear it is unstable caused by error；Accuracy high-precision is good, no
By being noiseless sample or disturbed specimen, measurement precision all with higher；
(3) there is wider linear test scope, fully meet the measurement of various content lead.
Specific embodiment
Below by a preferred embodiment of the present invention will be described in detail.The experiment of actual conditions is not specified in embodiment
Method, usually according to conventional conditions or according to the manufacturer's recommendations.
Embodiment 1
A method of the atomic absorption spectroscopy determination content of heavy metal lead without matrix modifier, including walk as follows
It is rapid:
(1) it prepares solution: preparing 0.5mol/L with the nitric acid and deionized water of excellent pure grade；With the nitric acid and top grade of excellent pure grade
Pure perchloric acid is matched according to the volume mixture of 9:1 is made mixed acid solution；
(2) prepare the lead standard solution of 100ng/mL: absorption product type is the lead single element mark of GBW (E) 080129
In quasi- substance 1.0mL to 100mL volumetric flask, nitric acid solution to the scale that the 0.5mol/L is added obtains the lead mark of 1.0 μ g/mL
Standard uses liquid, then draws in lead standard solution 10mL to the 100mL volumetric flask of 1.0 μ g/mL, and the nitre of the 0.5mol/L is added
Acid solution to scale obtains the lead standard solution of 100ng/mL；
(3) sample solution and blank reagent are prepared using dry resolution method: weighs sample 1.0000g in porcelain crucible, it is first small
Fire is carbonized in adjustable electric hot plate up to not smoldering, and is moved at 500 DEG C of Muffle furnace cooling after being ashed 7h；It is added 0.5mol/L's
Nitric acid solution by ash content dissolution moves back in volumetric flask, repeatedly wash porcelain crucible on a small quantity with deionized water, by washing lotion be merged into
In volumetric flask, then scale is settled to deionized water and obtains sample solution, prepare blank reagent with same dry resolution method；
(4) nitric acid solution of the lead standard solution and 0.5mol/L that take 100ng/mL described in step (2) is in graphite furnace
In automatic nearly sample device, executes graphite furnace and match mark method, the sample introduction composition of each point is respectively as follows :+20 μ L of the lead standard solution of 0 μ L
The nitric acid solution of 0.5mol/L, the nitric acid solution of 0.5mol/L of+18 μ L of the lead standard solution of 2 μ L, 4 μ L it is described
The nitric acid solution of the 0.5mol/L of+16 μ L of lead standard solution, the 0.5mol/L of+12 μ L of the lead standard solution of 8 μ L
Nitric acid solution, the nitric acid solution of 0.5mol/L of+8 μ L of the lead standard solution of 12 μ L, the lead standard of 16 μ L use
The nitric acid solution of the 0.5mol/L of+4 μ L of liquid, the heating procedure of graphite furnace are as shown in table 1.
1 graphite furnace heating procedure of table
| Serial number | Temperature (DEG C) | Time (sec) | Argon flow (L/min) |
| 1 | 60 | 3 | 0.10 |
| 2 | 120 | 20 | 0.10 |
| 3 | 250 | 10 | 0.10 |
| 4 | 450 | 5 | 1.00 |
| 5 | 450 | 10 | 1.00 |
| 6 | 450 | 3 | 0.00 |
| 7 | 1800 | 5 | 0.00 |
| 8 | 2500 | 2 | 1.00 |
The light absorption value for measuring each point obtains lead ion extinction according to plumbum ion concentration in lead standard solution and light absorption value
Value；It is again that ordinate obtains unary linear regression equation using plumbum ion concentration in lead standard solution as abscissa, light absorption value, such as
Shown in table 2.
The light absorption value of the lead standard solution test of 2 100ng/mL of table
(5) blank reagent and 20 μ L of sample solution prepared in aspiration step (3) respectively, injects graphite furnace, retest 3
The secondary light absorption value for obtaining blank reagent and sample solution, bring into step (4) unary linear regression equation calculate blank reagent with
The lead ion content of sample solution is as shown in table 2；
(6) according to " lead tolerance=(sample solution lead content-blank reagent lead content)/sample quality in every gram of sample "
Lead tolerance is as shown in table 2 in formula calculating sample, and the average value for taking last time to measure is to test lead ion content in every gram of sample.
Embodiment 2
A method of the atomic absorption spectroscopy determination content of heavy metal lead without matrix modifier, using embodiment
The unary linear regression equation that nitric acid solution, mixed acid solution and the test of 0.5mol/L in 1 obtains, and in the present embodiment
Sample solution and blank reagent are prepared using wet resolution method: weighing sample 1.0000g in conical flask, is put into bead, are added
The mixed acid solution soaked overnight of 15mL, in carrying out abatement on electric furnace or heating plate until solution becomes micro- yellow or transparent, resolution
Acid to white cigarette is caught up with to disperse；The hydrogen peroxide for being added 30% continues abatement to doing, and arrives capacity after the nitric acid solution of 0.5mol/L is added
In bottle and scale is settled to deionized water and obtains sample solution, prepares blank reagent with same wet resolution method；Then it inhales respectively
The blank reagent and 20 μ L of sample solution for taking step to prepare, inject graphite furnace, using identical heating procedure in embodiment 1, weight
Repetition measurement tries to obtain the light absorption value of blank reagent and sample solution 3 times, brings unary linear regression equation in step (4) into and calculates blank
The lead ion content of reagent and sample solution is as shown in table 3；According to " lead tolerance=(sample solution lead content-in every gram of sample
Blank reagent lead content)/sample quality " formula calculate sample in lead tolerance it is as shown in table 2, take last time measure average value be
Test lead ion content in every gram of sample.
The blank reagent of the dry resolution method of table 3 test and the lead ion content of sample solution
The reception standard of test are as follows: the absolute difference for the measurement result independent twice that precision obtains under the conditions of repeatability
It must not exceed the 20% of arithmetic mean of instantaneous value, and the relative deviation of dry resolution method and wet resolution method survey calculation is 10.7%, therefore
Meet and receive the requirement that standard is not more than 20%, illustrates that the measurement result of two kinds of digestion procedures is true and reliable.
The precision of measurement method detects:
6 duplicate measurements are carried out continuously to the lead standard solution that concentration is 10ng/mL and are recorded as a result, and arranging result
Enter table 4.
4 instrument precision of table (repeatability) result
| Detect number | Test value |
| 1 | 11.4783 |
| 2 | 10.7696 |
| 3 | 11.3455 |
| 4 | 11.0354 |
| 5 | 10.7696 |
| 6 | 11.5226 |
| RSD (%) | 3.07 |
The reception standard of precision are as follows: instrument precision must not exceed 6 repeated measuring results RSD of same contents level
5%, and the RSD value of the precision test result of this method is 3.07%, therefore meets and receive standard.
Intermediate precision detection:
The RSD value of test sample testing result at least three contents levels is measured, each contents level detects three times,
Three various concentration titers of addition under accuracy item are selected, accuracy is examined again in different time by second test person
It surveys, and result is included in table 5, it is known that concentration samples lead content is 0.1269ng/mL.
5 Intermediate precision result of table
Reception standard are as follows: pair and trace detection Intermediate precision result rate of recovery relative standard deviation be not more than 15%,
By measurement, RSD value is respectively 11.4%, 8.9%, meets and receives the requirement that standard is not more than 15%.
Accuracy detection:
With standard addition method, detected respectively three times on three contents levels.
Sample preparation: it takes sample precision to weigh 1 gram of sample, sample digestive juice is washed or filtered with dropper after dry method digestion
Enter in 100mL volumetric flask, as solution A.
Lead standard adds solution: drawing in 1 μ g/ml lead standard solution 1ml dilution and 100ml volumetric flask is (10ng/mL),
As solution B.
3 standard addition solution are prepared after the same method.
(1) B solution 1ml is accurately drawn in first bottle, acquired solution lead content are as follows: sample A lead content+10ng/mL.
(2) B solution 4ml is accurately drawn in second bottle, acquired solution lead content are as follows: sample A lead content+40ng/mL.
(3) B solution 8ml is accurately drawn in third bottle, acquired solution lead content are as follows: sample A lead content+80ng/mL.
According to examination requirements, instrument parameters are set, respectively sample introduction.And result is included in table 6.
Table 6: accuracy testing result
Note: the rate of recovery=(standardized sample concentration-sample solution concentration)/scalar quantity
Reception standard: pair and the trace detection rate of recovery should be between 80%-125%, result judgement: by measurement, recycling
Rate is 98.4%~122.4%, and average recovery rate is 107.9%, meets the requirement of reception standard 80%-125%.
Detection limit, quantitative limit detection:
Corresponding detectable concentration is used as quantitative limit when being usually 10 using signal-to-noise ratio (S/N), when with signal-to-noise ratio (S/N) being 3 pair
The detectable concentration answered is as detection limit.In the range of linearity as above on the basis of minimum concentration, standard solution is continued dilute
Measurement is released, its signal-to-noise ratio of test result is 0.3459.When signal-to-noise ratio (S/N) is 10, i.e., using this concentration as being quantitatively limited to 3ppb；
When signal-to-noise ratio (S/N) be 3, i.e., using this concentration as detect be limited to 1ppb.
Discussion of results
By fully meeting the measurement requirement of organic substance, symbol to linear, precision, Intermediate precision, accuracy detection
It closes it is anticipated that result.
Therefore by the test and analysis to indices, show that measuring method of the invention is applicable in trace element lead
Measurement, it has accuracy height and precision good, has very wide linear determination range, and detection process does not need addition matrix
A kind of effective ways for quickly measuring lead element may be implemented in modifier.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical
It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (10)
1. a kind of method of the atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier, which is characterized in that
The method is atomic absorption spectrophotometry, does not use matrix modifier in the method.
2. a kind of atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier according to claim 1
Method, which is characterized in that described method includes following steps:
(1) it prepares solution: preparing the nitric acid solution of 0.5mol/L and the nitric acid of 1mol/L with the nitric acid and deionized water of excellent pure grade
Solution；Matched with the nitric acid of excellent pure grade and the perchloric acid of excellent pure grade according to the volume mixture of 9:1 and mixed acid solution is made；
(2) it prepares the lead standard solution of 100ng/mL: utilizing the nitric acid solution and deionized water of the 0.5mol/L in step (1)
It prepares；
(3) sample solution and blank reagent are prepared using wet resolution method or dry resolution method: molten using the mixed acid in step (1)
The nitric acid solution of liquid and 0.5mol/L prepare sample solution, prepare blank reagent using process same as sample solution is prepared；
(4) light absorption value of the lead standard solution of atomic absorption spectroscopy determination 100ng/mL is utilized: in step (1)
The nitric acid solution of 0.5mol/L configures the lead standard solution to form different lead contents from the lead standard solution of 100ng/mL, uses
The light absorption value of the lead standard solution of atomic absorption spectroscopy determination difference lead content, then with lead in lead standard solution from
Sub- concentration is abscissa, corresponding light absorption value is that ordinate obtains unary linear regression equation；
(5) light absorption value of blank reagent and the light absorption value of sample solution are measured respectively using atomic absorption spectrophotometry, substitute into
The lead content of blank reagent and the lead content of sample solution are obtained in unary linear regression equation in step (4)；
(6) lead content in every gram of sample of sample is calculated.
3. a kind of atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier according to claim 2
Method, which is characterized in that mark method, the heating procedure of the graphite furnace are matched using graphite furnace in the atomic absorption spectrophotometry
As follows: a. is warming up to 60 DEG C within the time of 3s, while being passed through argon gas with the speed of 0.10L/min；B. it is risen within the time of 20s
Temperature is passed through argon gas to 120 DEG C, while with the speed of 0.10L/min；C. it is warming up to 250 DEG C within the time of 10s, while with
The speed of 0.10L/min is passed through argon gas；D. it is warming up to 450 DEG C within the time of 5s and keeps the temperature 10s, while with 1.00L/min's
Speed is passed through argon gas；E. 3s is kept the temperature at 450 DEG C in the case where obstructed argon gas；F. 1800 DEG C are warming up within the time of 5s；
G. it is warming up to 2500 DEG C within the time of 2s, while argon gas is passed through with the speed of 1.00L/min.
4. a kind of atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier according to claim 2
Method, which is characterized in that the preparation method of lead standard solution described in step (2) specifically: absorption product type is GBW
(E) in 080129 lead single element standard substance 1.0mL to 100mL volumetric flask, the nitric acid solution of the 0.5mol/L is added extremely
Scale obtains the lead standard solution of 1.0 μ g/mL, then draws lead standard solution 10mL to the 100mL volumetric flask of 1.0 μ g/mL
In, nitric acid solution to the scale that the 0.5mol/L is added obtains 100ng/mL lead standard solution.
5. a kind of atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier according to claim 2
Method, which is characterized in that wet resolution method described in step (3) prepares the specific steps of sample solution are as follows: weighs sample 1.0000g
In conical flask, it is put into bead, the mixed acid solution soaked overnight of 15mL is added, it is straight in carrying out cutting down on electric furnace or heating plate
Become micro- yellow or transparent to solution, resolution catches up with acid to white cigarette to disperse；The hydrogen peroxide for being added 30% continues abatement to dry, addition
Scale is settled to after the nitric acid solution of 0.5mol/L into volumetric flask and with deionized water.
6. a kind of atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier according to claim 2
Method, which is characterized in that the specific steps that resolution method prepares sample solution are done described in step (3) are as follows: weigh sample 1.0000g
In porcelain crucible, first small fire is carbonized in adjustable electric hot plate until do not smolder, move into ashing 6 at 475~525 DEG C of Muffle furnace~
It is cooling after 8h；The nitric acid solution that 0.5mol/L is added moves back ash content dissolution in volumetric flask, is repeatedly washed on a small quantity with deionized water
Porcelain crucible is washed, washing lotion is merged into volumetric flask, then is settled to scale with deionized water.
7. a kind of atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier according to claim 2
Method, which is characterized in that the test process of lead standard solution light absorption value described in step (4) are as follows: take described in step (2)
The lead standard solution of 100ng/mL and the nitric acid solution of 0.5mol/L execute graphite furnace with mark in graphite furnace automatically nearly sample device
Method, the sample introduction composition of each point are respectively as follows: the nitric acid solution of the 0.5mol/L of+20 μ L of the lead standard solution of 0 μ L, 2 μ
The nitric acid solution of the 0.5mol/L of+18 μ L of the lead standard solution of L ,+16 μ L of the lead standard solution of 4 μ L
The nitric acid solution of the 0.5mol/L, the nitric acid solution of the 0.5mol/L of+12 μ L of the lead standard solution of 8 μ L, 12 μ
The nitric acid solution of the 0.5mol/L of+8 μ L of the lead standard solution of L ,+4 μ L of the lead standard solution of 16 μ L
The nitric acid solution of the 0.5mol/L measures the light absorption value of each point with atomic absorption spectrophotometry.
8. a kind of atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier according to claim 2
Method, which is characterized in that the test process of blank reagent light absorption value described in step (5) are as follows: draw 20 μ L of blank reagent, injection
Graphite furnace measures its light absorption value with atomic absorption spectrophotometry.
9. a kind of atomic absorption spectroscopy determination content of heavy metal lead of no matrix modifier according to claim 2
Method, which is characterized in that the test process of the light absorption value of sample solution described in step (5) are as follows: 20 μ L of pipette samples solution, note
Enter graphite furnace, measures its light absorption value with atomic absorption spectrophotometry.
10. according to the atomic absorption spectroscopy determination content of heavy metal lead of a kind of no matrix modifier described in claim 2
Method, which is characterized in that the formula used in calculating described in step (6) are as follows: lead tolerance=(sample solution in every gram of sample
Lead content-blank reagent lead content)/sample quality.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811493888.1A CN109406429A (en) | 2018-12-07 | 2018-12-07 | A method of the atomic absorption spectroscopy determination content of heavy metal lead without matrix modifier |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811493888.1A CN109406429A (en) | 2018-12-07 | 2018-12-07 | A method of the atomic absorption spectroscopy determination content of heavy metal lead without matrix modifier |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109406429A true CN109406429A (en) | 2019-03-01 |
Family
ID=65457710
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811493888.1A Pending CN109406429A (en) | 2018-12-07 | 2018-12-07 | A method of the atomic absorption spectroscopy determination content of heavy metal lead without matrix modifier |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109406429A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111442960A (en) * | 2020-04-20 | 2020-07-24 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012063318A (en) * | 2010-09-17 | 2012-03-29 | Toppan Printing Co Ltd | Quantitative analysis method of trace titanium element |
| CN102608049A (en) * | 2011-10-14 | 2012-07-25 | 安徽皖仪科技股份有限公司 | Method for detecting aluminum in 2,2'-methylene-bis(4,6-di-bert-butyl phenol)phosphate |
| CN104408314A (en) * | 2014-11-27 | 2015-03-11 | 黑龙江省乳品工业技术开发中心 | Prediction method for lead content fading in lactation of dairy cow and application |
| CN104730010A (en) * | 2015-03-04 | 2015-06-24 | 嘉兴市产品质量检验检测院 | Method for detecting content of lead in zinc alloy button |
-
2018
- 2018-12-07 CN CN201811493888.1A patent/CN109406429A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012063318A (en) * | 2010-09-17 | 2012-03-29 | Toppan Printing Co Ltd | Quantitative analysis method of trace titanium element |
| CN102608049A (en) * | 2011-10-14 | 2012-07-25 | 安徽皖仪科技股份有限公司 | Method for detecting aluminum in 2,2'-methylene-bis(4,6-di-bert-butyl phenol)phosphate |
| CN104408314A (en) * | 2014-11-27 | 2015-03-11 | 黑龙江省乳品工业技术开发中心 | Prediction method for lead content fading in lactation of dairy cow and application |
| CN104730010A (en) * | 2015-03-04 | 2015-06-24 | 嘉兴市产品质量检验检测院 | Method for detecting content of lead in zinc alloy button |
Non-Patent Citations (4)
| Title |
|---|
| 中华人民共和国卫生部: "《食品安全标准 食品中铅的测定 GB5009.12-2010》", 26 March 2010 * |
| 孙汉文: "《原子光谱学与痕量分析研究》", 31 August 2001, 河北大学出版社 * |
| 朱洪法: "《催化剂手册》", 31 August 2008, 金盾出版社 * |
| 陈梦静 等: "石墨炉原子吸收测定铅含量中基体改进剂研究综述", 《现代农业科技》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111442960A (en) * | 2020-04-20 | 2020-07-24 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
| CN111442960B (en) * | 2020-04-20 | 2023-12-29 | 北京仪达仪器有限责任公司 | Kit and method for rapidly extracting heavy metals in soil |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101294896B (en) | Method for measuring cadmium content in smoke tipping paper | |
| CN101187629B (en) | Tobacco and tobacco product arsenic content determination method | |
| CN107192707A (en) | Arsenic, cadmium, copper, mercury, the method for the Heavy Metallic Elements of lead five in Bionic tiger bone powder are determined simultaneously | |
| CN103994994B (en) | The analysis method of silicon in vanadium iron | |
| CN101349639A (en) | Method for measuring mercury content in loading paper for cigarette | |
| CN110987918A (en) | Detection reagent and rapid detection method for total nitrogen in water | |
| CN103196849A (en) | Detection method of lead content in triacetin | |
| CN103529117A (en) | Measuring method for cobalt content in lining paper of cigarette | |
| CN110274882A (en) | Cadmium detrmination method in rice | |
| CN105910881B (en) | A kind of micromation heat auxiliary sample pretreatment device and application detected for Surface enhanced Raman spectroscopy | |
| CN109406429A (en) | A method of the atomic absorption spectroscopy determination content of heavy metal lead without matrix modifier | |
| CN101929992B (en) | Method for measuring oxidizable substance of drug packing material with total organic carbon analyser | |
| Horner et al. | Visible and infrared spectroscopic determination of trace amounts of silicones in foods and biological materials | |
| CN106018401A (en) | Method for determining content of chlorine ions in water | |
| CN113984693B (en) | Method for measuring residual quantity of harmful heavy metal in printing ink | |
| CN110530811A (en) | The analyzing detecting method of Cd metallic element in solid food sample | |
| CN110411817A (en) | The method of the direct mercury vapourmeter measurement mercury in hair content of DMA-80 | |
| CN105021692A (en) | Method for simultaneously determining multiple inorganic elements in cigarette liquid of electronic cigarette | |
| CN107991375A (en) | The kit of iodine in a kind of measure human urine | |
| Konieczka et al. | Utilization of thermal decomposition of immobilized compounds for the generation of gaseous standard mixtures used in the calibration of gas analysers | |
| CN103808708A (en) | Method for detecting components of industrial ammonium sulfate product | |
| CN113624700A (en) | Method for detecting p-nitrophenol | |
| CN106872427A (en) | H in a kind of carbon quantum dot targeting detection lysosome2The method of S | |
| CN111443056A (en) | Method for measuring mercury content in copper concentrate | |
| CN108507862A (en) | A kind of Cadmium detrmination method in animal's liver |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190301 |