CN103543142A - Method for detecting tin content in liquid - Google Patents
Method for detecting tin content in liquid Download PDFInfo
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- CN103543142A CN103543142A CN201310465518.8A CN201310465518A CN103543142A CN 103543142 A CN103543142 A CN 103543142A CN 201310465518 A CN201310465518 A CN 201310465518A CN 103543142 A CN103543142 A CN 103543142A
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Abstract
The invention provides a method for detecting tin content in a liquid and aims at overcoming the defects that a special reagent is used in a tin determination method in the prior art and sensitivity is low. The method for detecting the tin content in the liquid comprises the following concrete steps: A, preparing a tin standard solution, and adding a lanthanum solution into the tin standard solution; preparing a blank dilution solution, and adding the lanthanum solution into the blank dilution solution; preparing tin standard solutions in different concentrations; B, placing the tin standard solutions in different concentrations into a graphite furnace, determining absorbance of each standard solution, and making an absorbance-concentration standard curve; C, adding the lanthanum solution into a liquid sample to be detected, so as to prepare a sample solution; D, placing the sample solution into the graphite furnace, determining the absorbance of the sample solution, obtaining tin concentration of the sample solution, and calculating tin content in the sample solution. The method for detecting the tin content in the liquid has the advantages of high sensitivity, low detection limit, high accuracy, no use of special reagent and the like and is applicable to detection of tin content.
Description
Technical field
The present invention relates to the detection method of tenor in a kind of fluid sample, relate in particular to the detection method of tin content in a kind of liquid.
Background technology
Tin is one of indispensable trace element of human body, it carries out various physiological activities and safeguards that the health of human body has material impact people, and its main physiological function shows anti-tumor aspect, in addition, tin also promotes the synthetic of protein and nucleic acid, is conducive to growing of health; And the biological respinse that forms plurality of enzymes and participate in flavo-enzyme, can strengthen the stability of internal milieu etc.But people eat or suck too much tin, just likely occur dizzy, diarrhoea, nauseating, uncomfortable in chest, be short of breath, the ill symptoms such as dry, and cause Determination of Calcium in Serum content to reduce, when serious, also likely cause enterogastritis, and tin poisoning in industry can cause nervous system, liver function, mucocutaneous etc. suffering damage.
The assay method of tin mainly contains Phenylfuorone spectrophotometry and hydride generation---atomic fluorescence spectrometry at present, Phenylfuorone spectrophotometry need to be used a large amount of organic solvents, and operation steps is complicated, sensitivity is lower, detect and be limited to 10 μ g/L, can not meet the mensuration requirement of the fluid samples such as Drinking Water.Hydride occurs---AFS DETERMINATION tin, detect and be limited to 1 μ g/L, can meet the demands, but tin is very strict to the requirement of acidity, and need to use explosive hazardous chemical sodium borohydride, the chemicals of sodium borohydride Wei Shou public security department control, has limited popularization and the application of the method.
Summary of the invention
The present invention has overcome tin assay method complicated operation of the prior art, has used special reagent and the low shortcoming of sensitivity, and the detection method of tin content in a kind of liquid is provided.
The technical scheme that the present invention realizes goal of the invention employing is: the detection method of tin content in a kind of liquid, mainly configuration tin standard solution, drawing standard curve, sample pre-treatments, four steps of concentration that sample solution is detected to tin in calculation sample also, consist of, concrete steps are as follows:
A. configure tin standard solution: preparation tin standard solution, and add lanthanum solution in this tin standard solution; Prepare blank dilution, and add lanthanum solution in this blank dilution; With blank dilution, tin standard solution is diluted, prepare the tin standard solution of a plurality of variable concentrations;
B. drawing standard curve: the tin standard solution of a plurality of variable concentrations described in steps A is put to graphite furnace, by the absorbance of each standard solution of sampling Graphite Furnace Atomic Absorption spectrophotometric determination, made the typical curve of absorbance to concentration;
C. sample pre-treatments: add lanthanum solution in fluid sample to be measured, make sample solution;
D. sample solution is detected and calculation sample in the concentration of tin: the sample solution described in step C is put to graphite furnace, by the absorbance of sampling Graphite Furnace Atomic Absorption spectrophotometric determination sample solution, from the typical curve described in step B, obtain the tin concentration of sample solution, according to dilution ratio, calculate the tin content in sample solution, in sample solution, tin content is calculated as follows:
In formula: Abs-absorbance; The intercept of b---typical curve; The slope of k---typical curve; V
1---sample volume; V
2---constant volume.
Described lanthanum solution is prepared by lanthanum nitrate.
The ratio of the described lanthanum solution adding in this tin standard solution, the lanthanum solution adding in this blank dilution, the lanthanum solution that adds in fluid sample to be measured is identical.
The invention has the beneficial effects as follows: according to method provided by the invention, measure the tin content in fluid sample, operation steps is simple, highly sensitive, detect and be limited to 0.6 μ g/L, lower than hydride, occur---the detection limit of atomic fluorescence spectrometry, the general reagent that the reagent lanthanum nitrate using in testing process is non-control, and add lanthanum nitrate can with sample in tin form alloy, eliminated the volatilization of tin in graphite furnace heating process, guaranteed the accuracy of result, have highly sensitive, detection limit is low, accuracy is good, simple to operate, do not use special reagent etc. advantage, applicable to Drinking Water and source water thereof, surface water, underground water, industrial waste water, sanitary wastewater, the mensuration of tin content in the fluid samples such as seawater.
Below in conjunction with accompanying drawing and embodiment, the invention will be further described.
Accompanying drawing explanation
Fig. 1 is method flow diagram of the present invention.
Fig. 2 is the typical curve of tin element absorbance of the present invention to concentration.
Embodiment
As shown in Figure 1, the detection method of tin content in a kind of liquid of the present embodiment, mainly configuration tin standard solution, drawing standard curve, sample pre-treatments, four steps of concentration that sample solution is detected to tin in calculation sample also, consist of, concrete steps are as follows:
A. configure tin standard solution: preparation tin standard solution, and add lanthanum solution in this tin standard solution, the concentration of the preferred tin standard solution of the present embodiment is 100 μ g/L, and guarantees in every 100mL standard solution to be 30g/L lanthanum solution containing 5mL concentration; Prepare blank dilution, and add lanthanum solution in this blank dilution, and guarantee that in the blank dilution of every 100mL be 30g/L lanthanum solution containing 5mL concentration; With blank dilution, tin standard solution is diluted, microsyringe, according to the sample size dosage shown in following table, prepares the tin standard solution of a plurality of variable concentrations,
| The actual tin concentration of solution (μ g/L) | 0 | 10 | 20 | 30 | 50 |
| Tin standard solution addition (μ L) | 0 | 2 | 4 | 6 | 10 |
| Blank dilution addition (μ L) | 20 | 18 | 16 | 14 | 10 |
B. drawing standard curve: the tin standard solution of a plurality of variable concentrations described in steps A 20 μ L are put to graphite furnace, by the absorbance of each standard solution of sampling Graphite Furnace Atomic Absorption spectrophotometric determination, the running parameter of the atomic absorption spectrophotometer of the present embodiment is set as according to Shimadzu AA-7000 instrument:
| Element | Tin |
| Wavelength (nm) | 286.3 |
| Lamp current Low(peak value) (mA) | 15 |
| Slit wide (nm) | 0.7 |
| The mode of lighting a lamp | BGC-D2 |
If the instrument of other model or the instrument of other company production that adopt Shimadzu company to produce, should revise according to the operation instructions of instrument,
The graphite furnace condition of work of the present embodiment is:
Graphite furnace running parameter can optionally be used on the instrument of different company and different model;
Measurement result sees the following form,
By the absorbance recording, be ordinate, the actual tin concentration of solution is horizontal ordinate, makes the typical curve of absorbance to concentration, as shown in Figure 2;
C. sample pre-treatments: fluid sample 90mL to be measured is added in 100mL volumetric flask, and adding 5mL concentration is the lanthanum solution of 30g/L, is settled to scale, makes sample solution;
D, to sample solution detect and calculation sample in the concentration of tin: the 20 μ L of the sample solution described in step C are put to graphite furnace, by the absorbance of sampling Graphite Furnace Atomic Absorption spectrophotometric determination sample solution, from the typical curve described in step B, obtain the tin concentration of sample solution, according to dilution ratio, calculate the tin content in sample solution, in sample solution, tin content is calculated as follows:
In formula: Abs-absorbance; The intercept of b-typical curve ,-0.001; The slope of k-typical curve, 0.011; V
1-sample volume, mL; V
2-constant volume, mL.
The tin content of measuring in the present invention is the trace level of μ g/L, and tin or other heavy metal pollution will affect measurement result, therefore the container and the pure water that use in steps should guarantee not have tin or other heavy metal pollution.Volumetric flask used is glass material, and grade is A level, and before using, application 10% salpeter solution soaks more than 8 hours, and with pure water drip washing 3 times.Drip washing and the pure water resistivity adding should guarantee to be greater than 18.2M Ω/cm.
Because this method is to carry out heating sample with graphite furnace, if contain the negative ion such as a large amount of chlorions, sulfate ion, phosphate radical in sample, can produce negative interference to measurement result, so the lanthanum solution of the present embodiment is prepared by lanthanum nitrate.
The ratio of the lanthanum solution adding in this tin standard solution, the lanthanum solution adding in this blank dilution, the lanthanum solution that adds in fluid sample to be measured is identical, as diluted again, the ratio that should guarantee the lanthanum solution that adds is identical, the lanthanum solution that it is 30g/L containing 5mL concentration in every 100mL solution that the present embodiment should be guaranteed.
Specifically describe the collocation method of part solution below:
The preparation of (1) 1% salpeter solution
Get the pure nitric acid 10.0mL of commercially available top grade, add in 1000mL volumetric flask, with pure water, be settled to scale.
(2) preparation of tin standard solution
The preparation of tin standard intermediate liquid: get commercially available tin national standard solution, concentration is 1000 μ g/mL, accurately draws 10.0mL tin standard solution, adds in 1000mL volumetric flask, is settled to scale with 1% salpeter solution, in this solution, tin content is 10 μ g/mL.
The preparation of tin standard solution: accurately draw 10.0mL tin standard intermediate liquid, add in 1000mL volumetric flask, adding 50mL concentration is the lanthanum solution of 30g/L, is settled to scale with 1% salpeter solution, and in this solution, tin content is 100 μ g/L.
(3) preparation of the lanthanum solution that concentration is 30g/L
Accurately take the pure lanthanum nitrate of 9.35g top grade [La (NO
3)
36H
2o], with 1% salpeter solution, be settled to 100mL.
(4) preparation of blank dilution
Accurately draw the lanthanum solution that 5mL concentration is 30g/L, with 1% salpeter solution, be settled to 100mL.
The Precision Experiment that this method is measured stanniferous fluid sample is:
In Shenzhen, randomly draw Drinking Water sample, be divided into 6 parts, every part of 100mL, 2 parts of each minutes, every part of 50mL.In 1 part of solution, add tin standard solution 30mL therein, then to add 5mL concentration be the lanthanum solution of 30g/L, be settled to 100mL, totally 6 parts is the 1st group of sample, and mark-on concentration is 30 μ g/L.In another part of solution, adding 5mL concentration is the lanthanum solution of 30g/L, is settled to 100mL, and totally 6 parts is the 2nd group of sample.
Add successively the 1st group and the 2nd group of sample 20 μ L to graphite furnace.Start graphite furnace control program, measure the absorbance of each sample solution, from typical curve, directly check in the tin concentration sample solution, result is as shown in the table,
Drinking Water mark-on test findings
As can be seen from the above table, in mensuration fluid sample provided by the invention, the method for tin content is applicable to the mensuration of tin content in the fluid samples such as Drinking Water and source water thereof, surface water, underground water, industrial waste water, sanitary wastewater, seawater completely, the recovery is between 90-110%, relative standard deviation is less than 10%, result precision is high, reproducible.
Claims (3)
1. a detection method for tin content in liquid, is mainly comprised of configuration tin standard solution, drawing standard curve, sample pre-treatments, four steps of concentration that sample solution is detected to tin in calculation sample also, it is characterized in that, concrete steps are as follows:
A. configure tin standard solution: preparation tin standard solution, and add lanthanum solution in this tin standard solution; Prepare blank dilution, and add lanthanum solution in this blank dilution; With blank dilution, tin standard solution is diluted, repeat the tin standard solution that above-mentioned steps prepares a plurality of variable concentrations;
B. drawing standard curve: the tin standard solution of a plurality of variable concentrations described in steps A is put to graphite furnace, by the absorbance of each standard solution of sampling Graphite Furnace Atomic Absorption spectrophotometric determination, made the typical curve of absorbance to concentration;
C. sample pre-treatments: add lanthanum solution in fluid sample to be measured, make sample solution;
D, to sample solution detect and calculation sample in the concentration of tin: the sample solution described in step C is put to graphite furnace, by the absorbance of sampling Graphite Furnace Atomic Absorption spectrophotometric determination sample solution, from the typical curve described in step B, obtain the tin concentration of sample solution, according to dilution ratio, calculate the tin content in sample solution, in sample solution, tin content is calculated as follows:
In formula: Abs-absorbance; The intercept of b-typical curve; The slope of k-typical curve; V
1-sample volume; V
2-constant volume.
2. the detection method of tin content in a kind of liquid according to claim 1, is characterized in that, described lanthanum solution is prepared by lanthanum nitrate.
3. the detection method of tin content in a kind of liquid according to claim 1, it is characterized in that, the ratio of the described lanthanum solution adding in this tin standard solution, the lanthanum solution adding in this blank dilution, the lanthanum solution that adds in fluid sample to be measured is identical.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115389435A (en) * | 2022-09-01 | 2022-11-25 | 深圳市迈启生物材料有限公司 | Method for detecting content of tin in polylactic acid |
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Application publication date: 20140129 |