CN107632013A - The assay method of arsenogen cellulose content in a kind of tin sample - Google Patents
The assay method of arsenogen cellulose content in a kind of tin sample Download PDFInfo
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- CN107632013A CN107632013A CN201710640650.6A CN201710640650A CN107632013A CN 107632013 A CN107632013 A CN 107632013A CN 201710640650 A CN201710640650 A CN 201710640650A CN 107632013 A CN107632013 A CN 107632013A
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Abstract
The present invention discloses a kind of assay method of arsenogen cellulose content in tin sample, and the assay method comprises the following steps：1) the tin sample is dissolved using the first hydrochloric acid solution and hydrogenperoxide steam generator, after adding the second hydrochloric acid solution, is diluted with water, obtains sample solution；2) liquor kalii iodide, stannous chloride solution and zinc granule are added in the sample solution obtained to the step 1), reaction produces mixed gas；The mixed gas includes arsine gas；3) absorbing liquid reactive absorption is used to arsine gas caused by the step 2), adds chloroform；Obtain solution to be measured；4) standard working curve is established；Reference is made with chloroform, determines the absorbance of solution absorbance and blank solution to be measured that the step 3) obtains, arsenic amount and the arsenic amount of blank solution in solution to be measured are obtained according to standard working curve, arsenogen cellulose content in tin sample is calculated；The assay method is simple to operate, and test accuracy is high.
Description
Technical field
The present invention relates to analysis and testing technology field, and in particular to the assay method of arsenogen cellulose content in a kind of tin sample.
Background technology
China's Tin Resources very abundant, the proved reserves of tin ore are 26,000,000 tons, account for the 1/4 of world's proved reserves, are
The most country of tin ore proved reserves in the world.The tin ore strategic resource important as China, it is widely used, containing more in tin sample
Kind impurity element, affect industrial use expansion.
In high purity tin the analysis of impurity content at present commonly use iodometric determination, influence of the tin main body to dirt content test compared with
Greatly, measurement result is inaccurate.
The content of the invention
In view of this, this application provides a kind of assay method of arsenogen cellulose content in tin sample, the assay method operation
Simply, the degree of accuracy of arsenic element assay is high in tin sample.
To solve above technical problem, technical scheme provided by the invention is a kind of measure side of arsenogen cellulose content in tin sample
Method, the assay method comprise the following steps：
1) the tin sample is dissolved using the first hydrochloric acid solution and hydrogenperoxide steam generator, after adding the second hydrochloric acid solution, adds water
Dilution, obtains sample solution；
2) liquor kalii iodide, stannous chloride solution and zinc granule, reaction are added in the sample solution obtained to the step 1)
Produce mixed gas；The mixed gas includes arsine gas；
3) arsine gas caused by the step 2) uses arsenic absorbing liquid reactive absorption, adds chloroform；Obtain to be measured molten
Liquid；
4) standard working curve is established；Reference is made with chloroform, determine solution absorbance to be measured that the step 3) obtains and
The absorbance of blank solution, arsenic amount and the arsenic amount of blank solution in solution to be measured are obtained according to standard working curve, are calculated
Arsenogen cellulose content in tin sample.
Preferably, arsenogen cellulose content is calculated as follows to obtain in the tin sample：
In formula：
X is that arsenogen cellulose content in the tin sample, numerical value is represented with % in terms of mass fraction；m1It is bent to be worked according to standard
Line obtains arsenic amount in solution to be measured, and unit is μ g；m2To obtain arsenic amount in blank solution, unit μ according to standard working curve
g；m0For the weight of the tin sample, unit g.
Preferably, the first concentration of hydrochloric acid solution described in the step 1) is concentrated hydrochloric acid, and the hydrogenperoxide steam generator is full
And solution, second hydrochloric acid solution are 1：1.
Preferably, the step 2) is specially：Added in the sample solution that the step 1) obtains 1ml liquor kalii iodides,
3ml stannous chloride solutions, 10min is vibrated, add 5g zinc granules, reaction produces arsine gas.
It is furthermore preferred that the step 2) is specially：The sample solution that the step 1) obtains is placed in generating bottle, the examination
1ml liquor kalii iodides, 3ml stannous chloride solutions are added in sample solution, vibrates 10min, adds 5g zinc granules, reaction produces gaseous mixture
Body；The mixed gas includes arsine gas.Preferably, the step 2) the liquor kalii iodide concentration is 150g/l, institute
Stannous chloride solution is stated by 10gSnCl2·2H2O is dissolved in 100ml hydrochloric acid 1：1 preparation obtains.
Preferably, hydrogen sulfide gas is also included in the mixed gas；The mixed gas is passed through into dry lead acetate
After cotton removes hydrogen sulfide gas therein, then with arsenic absorbing liquid reactive absorption arsine gas therein.Preferably, the vinegar
Lead plumbate cotton after acetic acid lead solution soaks, is prepared by absorbent cotton in 100 DEG C of drying.
Preferably, the step 3) is specially：Arsine gas caused by the step 2) is reacted using 6ml arsenic absorbing liquid
Absorb, add 6ml chloroforms；Obtain solution to be measured.
Preferably, the reactive absorption time described in the step 3) is 45~55min.
Preferably, in the step 3) arsenic absorbing liquid by 1.25g Silver diethydithiocarbamates, 500ml chloroforms and
15ml triethanolamines mix, and stand, are filtrated to get.
Preferably, in the step 4), the solution extinction to be measured that the step 3) obtains is determined under 510nm wavelength conditions
The absorbance of degree and blank solution.
Preferably, in the step 4), using 2cm absorption cells determine solution absorbance to be measured that the step 3) obtains and
The absorbance of blank solution.
Preferably, it is calculated in mass percent, Theil indices are not less than 99.999% in the tin sample.
Preferably, it is calculated in mass percent, arsenogen cellulose content is 1 × 10 in the tin sample-5%~5 × 10-3%.
Preferably, the standard working curve process of establishing is specially：Arsenic standard working solution is taken, adds second hydrochloric acid
Afterwards, one group of arsenic element gradation standard solution is prepared；Liquor kalii iodide, stannous chloride are added in the arsenic element gradation standard solution
Solution and zinc granule, react generation standard under test gas；The standard under test gas includes arsenic hydride；The standard under test gas is adopted
With arsenic absorbing liquid reactive absorption, chloroform is added, obtains one group of arsenic element gradation standard solution to be measured；Reference is made with chloroform, determined
Arsenic element gradation standard solution absorbance to be measured and blank solution absorbance, using arsenic quality as abscissa, it is molten to deduct blank
The arsenic element gradation standard solution absorbance to be measured of the absorbance of liquid is ordinate, drawing curve.
Compared with prior art, its detailed description is as follows by the application：
Continuous mode of the present invention is completely dissolved tin sample using the first hydrochloric acid solution and hydrogenperoxide steam generator, adds the second hydrochloric acid
Solution.Ensure that tin sample is completely dissolved；Avoid arsenic volatilization loss；Make sample solution into acidity, sample is molten under conditions of certain acidity
Pentavalent arsenic in liquid is reduced to trivalent arsenic under KI and stannous chloride effect, obtains arsenic trioxide, arsenic trioxide with
Zinc further reacts generation arsenic hydride, and arsenic hydride acts on the silver diethyl dithio carbamate in arsenic absorbing liquid, organic
In the presence of alkali triethanolamine, generation red colloid silver, the depth of color is directly proportional to arsenogen cellulose content in tin sample, available for colorimetric
Measure, and accuracy of measurement is high.
The present invention removes the hydrogen sulfide gas in mixed gas using lead acetate cotton, avoids measuring arsenic in solution to be measured
The interference of amount, the degree of accuracy of arsenic element assay is high in tin sample.
Continuous mode of the present invention is simple to operate, controllable, and reagent dosage is few.
Embodiment
In order that those skilled in the art more fully understands technical scheme, with reference to specific embodiment pair
The present invention is described in further detail.
The assay method of arsenogen cellulose content, the assay method comprise the following steps in a kind of tin sample：
1) the tin sample is dissolved using the first hydrochloric acid solution and hydrogenperoxide steam generator, after adding the second hydrochloric acid solution, adds water
Dilution, obtains sample solution；
2) liquor kalii iodide, stannous chloride solution and zinc granule, reaction production are added in the sample solution that the step 1) obtains
Raw mixed gas；The mixed gas includes arsine gas；
3) arsine gas caused by the step 2) uses arsenic absorbing liquid reactive absorption, adds chloroform；Obtain to be measured molten
Liquid；
4) standard working curve is established；Reference is made with chloroform, determine solution absorbance to be measured that the step 3) obtains and
The absorbance of blank solution, arsenic amount and the arsenic amount of blank solution in solution to be measured are obtained according to standard working curve, are calculated
Arsenogen cellulose content in tin sample.
According to the present invention, arsenogen cellulose content is calculated as follows to obtain in the tin sample：
In formula：
X is that arsenogen cellulose content in the tin sample, numerical value is represented with % in terms of mass fraction；m1It is bent to be worked according to standard
Line obtains arsenic amount in solution to be measured, and unit is μ g；m2To obtain arsenic amount in blank solution, unit μ according to standard working curve
g；m0For the weight of the tin sample, unit g.
It is concentrated hydrochloric acid to the first concentration of hydrochloric acid solution described in the step 1) according to the present invention, the hydrogen peroxide is molten
Liquid is saturated solution, and second hydrochloric acid solution is 1：1.
According to the present invention, the step 2) is specially：It is molten that 1ml KIs are added in the sample solution that the step 1) obtains
Liquid, 3ml stannous chloride solutions, 10min is vibrated, add 5g zinc granules, reaction produces arsine gas.Preferably, the step 2)
Specially：The sample solution that the step 1) obtains is placed in generating bottle, added in the sample solution 1ml liquor kalii iodides,
3ml stannous chloride solutions, 10min is vibrated, add 5g zinc granules, reaction produces mixed gas, and the mixed gas includes arsenic hydride
Gas.The liquor kalii iodide concentration is 150g/l, and the stannous chloride solution is by 10gSnCl2·2H2O is dissolved in 100ml hydrochloric acid
(1：1) prepare and obtain.
According to the present invention, it is preferred that also included hydrogen sulfide in mixed gas caused by described；By caused arsenic hydride gas
Body removes hydrogen sulfide gas by dry lead acetate cotton pipeline absorber.
According to the present invention, the step 3) is specially：Arsine gas caused by the step 2) uses 6ml arsenic absorbing liquids
Reactive absorption, add 6ml chloroforms；Obtain solution to be measured.Preferably, the step 3) is specially：Arsenic caused by the step 2)
Change hydrogen and enter reactive absorption in the absorption tube for filling 6ml arsenic absorbing liquids through connecting tube, add 6ml chloroforms；Obtain to be measured molten
Liquid.One section of dry lead acetate cotton is arranged in the connecting tube.Preferably, the lead acetate cotton by absorbent cotton through lead acetate
After solution soaks, it is prepared in 100 DEG C of drying.It is furthermore preferred that the acetic acid lead solution by 4g lead acetates, 2ml acetic acid and
100ml water mixes, and is prepared.
According to the present invention, the reactive absorption time described in the step 3) is 45~55min.Arsenic absorbing liquid is by 1.25g bis-
Ethylamino dithiocarbonic acid silver, 500ml chloroforms and the mixing of 15ml triethanolamines, stand, are filtrated to get.
According to the present invention, in the step 4), the solution to be measured that the step 3) obtains is determined under 510nm wavelength conditions
The absorbance of absorbance and blank solution.In the step 4), obtained using the 2cm absorption cells measure step 3) to be measured molten
The absorbance of liquid absorbance and blank solution.
According to the present invention, it is calculated in mass percent, Theil indices are not less than 99.999% in the tin sample.
According to the present invention, it is calculated in mass percent, arsenogen cellulose content is 1 × 10 in the tin sample-5%~5 × 10-3%.
According to the present invention, the standard working curve process of establishing is specially：Arsenic standard working solution is taken, adds second salt
After acid, one group of arsenic element gradation standard solution is prepared；Liquor kalii iodide, dichloride are added in the arsenic element gradation standard solution
Solution of tin and zinc granule, reaction produce arsine gas；The arsine gas uses arsenic absorbing liquid reactive absorption, adds chloroform,
Obtain one group of arsenic element gradation standard solution to be measured；Reference is made with chloroform, arsenic element gradation standard solution to be measured is determined and inhales
Luminosity and blank solution absorbance, using arsenic quality as abscissa, the arsenic element gradation standard for deducting the absorbance of blank solution is treated
Survey solution absorbance is ordinate, drawing curve.
Embodiment
First hydrochloric acid：Concentrated hydrochloric acid；
Hydrogenperoxide steam generator：Saturation hydrogenperoxide steam generator；
Second hydrochloric acid solution：For hydrochloric acid (1：1)；
Liquor kalii iodide：Concentration is 150g/l；
Stannous chloride solution：By 10gSnCl2·2H2O be dissolved in 100ml (1+1) hydrochloric acid prepare to obtain the stannous chloride it is molten
Liquid；
Arsenic absorbing liquid：Mixed by 1.25g Silver diethydithiocarbamates, 500ml chloroforms and 15ml triethanolamines, vibration
To dissolving, stand overnight, be filtrated to get；
Acetic acid lead solution：Mixed, be prepared by 4g lead acetates, 2ml acetic acid and 100ml water；
Lead acetate cotton：By absorbent cotton after acetic acid lead solution soaks, it is prepared in 100 DEG C of drying；
Arsenic standard working solution：It is 1mg/ml arsenic Standard Stock solutions to take arsenic content, is mixed with 5mlHCl and is settled to 100ml,
Obtain the arsenic standard working solution that arsenic content is 5ug/ml.
The assay method of arsenogen cellulose content, the assay method comprise the following steps in a kind of tin sample：
1.000g tin samples are taken to be placed in 100ml beakers, heating water bath beaker, the addition hydrochloric acid solutions of 10ml first, dropwise addition 2~
3ml hydrogenperoxide steam generators dissolve tin sample, after adding the hydrochloric acid solutions of 5ml second, move into generating bottle, are diluted with water to 30ml, obtain
To sample solution；It is calculated in mass percent, Theil indices are not less than 99.999% in the tin sample；
1ml liquor kalii iodides, 3ml stannous chloride solutions are added in the sample solution, vibrates 10min, adds 5g zinc granules,
Reaction produces mixed gas；The mixed gas includes arsine gas；Mixed gas is passed through provided with dry vinegar caused by described
Enter after the connecting tube of lead plumbate cotton and fill 6ml arsenic absorbing liquid 45~55min of reactive absorption, add 6ml chloroforms；Obtain to be measured molten
Liquid；
Establish standard working curve：0.0ug, 0.5ug, 1.0ug, 2.0ug, 3.0ug arsenic standard working solution are taken, adds 10ml institutes
After stating the second hydrochloric acid, one group of arsenic element gradation standard solution is prepared；Iodine described in 1ml is added in the arsenic element gradation standard solution
Stannous chloride solution described in change potassium solution, 3ml, vibrates 10min, adds 5g zinc granules, reacts generation standard under test gas；The mark
Quasi- under test gas includes arsenic hydride；The standard under test gas uses 6ml arsenic absorbing liquid reactive absorption 45min, adds 6ml chlorine
It is imitative, obtain one group of arsenic element gradation standard solution to be measured；Reference is made with chloroform, 2cm absorption cells, under the conditions of 510nm wavelength conditions,
Arsenic element gradation standard solution absorbance to be measured and blank solution absorbance are determined, using arsenic quality as abscissa, is deducted empty
The arsenic element gradation standard solution absorbance to be measured of the absorbance of white solution is ordinate, drawing curve；
Reference is made with chloroform, 2cm absorption cells, under the conditions of 510nm wavelength conditions, determine the step 3) obtain it is to be measured molten
The absorbance of liquid absorbance and blank solution, the arsenic of arsenic amount and blank solution in solution to be measured is obtained according to standard working curve
Amount, is calculated as follows to obtain arsenogen cellulose content in tin sample.
In formula：
X is that arsenogen cellulose content in the tin sample, numerical value is represented with % in terms of mass fraction；m1It is bent to be worked according to standard
Line obtains arsenic amount in solution to be measured, and unit is μ g；m2To obtain arsenic amount in blank solution, unit μ according to standard working curve
g；m0For the weight of the tin sample, unit g.
It the above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
The limitation of the present invention, protection scope of the present invention should be defined by claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Enter and retouch and also should be regarded as protection scope of the present invention.
Claims (10)
1. the assay method of arsenogen cellulose content in a kind of tin sample, it is characterised in that the assay method comprises the following steps：
1) the tin sample is dissolved using the first hydrochloric acid solution and hydrogenperoxide steam generator, after adding the second hydrochloric acid solution, is diluted with water,
Obtain sample solution；
2) liquor kalii iodide, stannous chloride solution and zinc granule are added in the sample solution obtained to the step 1), reaction produces
Mixed gas；The mixed gas includes arsine gas；
3) arsenic absorbing liquid reactive absorption is used to arsine gas caused by the step 2), adds chloroform；Obtain solution to be measured；
4) standard working curve is established；Reference is made with chloroform, determines solution absorbance to be measured and blank that the step 3) obtains
The absorbance of solution, arsenic amount and the arsenic amount of blank solution in solution to be measured are obtained according to standard working curve, tin sample is calculated
Middle arsenogen cellulose content.
2. detection method according to claim 1, it is characterised in that arsenogen cellulose content is calculated as follows in the tin sample
Arrive：
<mrow>
<mi>X</mi>
<mo>=</mo>
<mfrac>
<mrow>
<msub>
<mi>m</mi>
<mn>1</mn>
</msub>
<mo>-</mo>
<msub>
<mi>m</mi>
<mn>2</mn>
</msub>
</mrow>
<mrow>
<msub>
<mi>m</mi>
<mn>0</mn>
</msub>
<mo>&times;</mo>
<msup>
<mn>10</mn>
<mn>6</mn>
</msup>
</mrow>
</mfrac>
<mo>&times;</mo>
<mn>100</mn>
<mi>%</mi>
</mrow>
In formula：
X is that arsenogen cellulose content in the tin sample, numerical value is represented with % in terms of mass fraction；m1To be obtained according to standard working curve
Arsenic amount in solution to be measured, unit are μ g；m2To obtain arsenic amount in blank solution according to standard working curve, unit is μ g；m0For institute
State the weight of tin sample, unit g.
3. assay method according to claim 1, it is characterised in that the step 1) is specially：1.000g tin samples are taken, are added
Enter the hydrochloric acid solutions of 10ml first, 2~3ml hydrogenperoxide steam generators dissolving tin sample is added dropwise, after adding the hydrochloric acid solutions of 5ml second, adds water
30ml is diluted to, obtains sample solution.
4. assay method according to claim 1, it is characterised in that the first hydrochloric acid solution described in the step 1) is dense
Hydrochloric acid, the hydrogenperoxide steam generator are saturation hydrogenperoxide steam generator, and second hydrochloric acid solution is 1：1.
5. assay method according to claim 1, it is characterised in that be specially to the step 2)：The step 1)
To sample solution in add 1ml liquor kalii iodides, 3ml stannous chloride solutions, vibrate 10min, add 5g zinc granules, reaction produces
Mixed gas；The mixed gas includes arsine gas.
6. assay method according to claim 1, it is characterised in that step 2) the liquor kalii iodide concentration is
150g/l, the stannous chloride solution is by 10gSnCl2·2H2O is dissolved in 100ml hydrochloric acid (1:1) prepare and obtain.
7. assay method according to claim 1, it is characterised in that also include hydrogen sulfide gas in the mixed gas；
After the mixed gas is removed into hydrogen sulfide gas therein by dry lead acetate cotton, then with arsenic absorbing liquid reactive absorption
Arsine gas therein.
8. assay method according to claim 1, it is characterised in that the step 3) is specially：The step 2) produces
Arsine gas use 6ml arsenic absorbing liquid reactive absorptions, add 6ml chloroforms；Obtain solution to be measured.
9. assay method according to claim 1, it is characterised in that arsenic absorbing liquid is by 1.25g diethyls in the step 3)
Aminodithioformic acid silver, 500ml chloroforms and the mixing of 15ml triethanolamines, stand, are filtrated to get.
10. assay method according to claim 1, it is characterised in that be calculated in mass percent, Theil indices in the tin sample
Not less than 99.999%.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102841068A (en) * | 2012-09-19 | 2012-12-26 | 白银有色集团股份有限公司 | Method for analyzing and determining bismuth content in pure lead |
| CN105136765A (en) * | 2015-09-24 | 2015-12-09 | 神华集团有限责任公司 | Method of determining content of arsenic element in coal-containing sample |
-
2017
- 2017-07-31 CN CN201710640650.6A patent/CN107632013A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102841068A (en) * | 2012-09-19 | 2012-12-26 | 白银有色集团股份有限公司 | Method for analyzing and determining bismuth content in pure lead |
| CN105136765A (en) * | 2015-09-24 | 2015-12-09 | 神华集团有限责任公司 | Method of determining content of arsenic element in coal-containing sample |
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| 刘廷良等: "《中华人民共和国国家标准 GB/T 17134-1997 土壤质量 总砷的测定 二乙基二硫代氨基甲酸银分光光度法》", 1 May 1998 * |
| 刘清: "微波溶样用于化妆品中铅、汞、砷的测定 ", 《甘肃中医学院学报》 * |
| 刘清: "微波溶样用于化妆品中铅、汞、砷的测定", 《甘肃中医学院学报》 * |
| 王婷等: "《中华人民共和国国家标准GB／T 6276.7-2010工业用碳酸氢铵的测定方法第7部分：砷含量 二乙基二硫代氨基甲酸银分光光度法》", 30 June 2010 * |
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