CN104914093A - Method for testing constant cadmium and zinc in cadmium zinc telluride crystal - Google Patents
Method for testing constant cadmium and zinc in cadmium zinc telluride crystal Download PDFInfo
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- CN104914093A CN104914093A CN201410091151.2A CN201410091151A CN104914093A CN 104914093 A CN104914093 A CN 104914093A CN 201410091151 A CN201410091151 A CN 201410091151A CN 104914093 A CN104914093 A CN 104914093A
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Abstract
The invention provides a method for testing constant cadmium and zinc in cadmium zinc telluride crystal. The method provided by the invention comprises the following steps: taking a solution obtained by dissolving a proper amount of a sample solution of the cadmium zinc telluride crystal to be tested or a proper amount of a solid sample of the cadmium zinc telluride crystal to be tested, adjusting pH value of the solution to neutral by adding ammoniacal liquor (1+1) to and adjusting pH value of the solution to 10 by adding a proper amount of an ammonia-ammonium chloride buffer solution and remaining stable; adding a proper amount of a surfactant into the solution, adding a proper amount of an eriochrome black T indicator, and carrying out complexometric titration by the use of a complexing agent EDTA to turn the solution from purple to pure blue so as to obtain total amount nCd+Zn of cadmium and zinc, wherein molar concentration of the complexing agent EDTA is C1 and the use amount is V1; adding a proper amount of DDTC sodium salt to fully dissolve, selectively precipitate cadmium by DDTC sodium salt and releasing the same amount of EDTA, carrying out titration on EDTA by the use of a magnesium nitrate solution until the solution turns light red so as to obtain cadmium with the amount of nCd and mass of mCd, wherein molar concentration of the magnesium nitrate solution is C2 and use amount is V2; and obtaining zinc with amount of nZn and mass of mZn according to a difference method.
Description
Technical field
The present invention relates to chemical analysis method field, particularly relate to the method for testing of constant cadmium and zinc in a kind of tellurium-zincium-cadmium crystal.
Background technology
Tellurium zinc cadmium (Cd
1-xzn
xte, is abbreviated as CZT) monocrystal is a kind of ternary semiconductor indoor temperature nucleus radiation detector material of excellent performance, is widely used in the fields such as nuclear safety, environmental monitoring, astrophysics and medical imaging.At present, CZT detector becomes one of focus of countries in the world research.In CZT monocrystal, the difference of Cd and Zn content can the performance of appreciable impact CZT monocrystal, and therefore the content of Cd and Zn in Accurate Determining CZT, is one of key of the CZT monocrystal of synthesis particular characteristic.
The common method measuring the content of cadmium and zinc has disodium ethylene diamine tetraacetate (EDTA) compleximetry, strong base difference titrimetry, potassium iodide replacement titration, potassium iodide-sulfosalicylic acid replacement titration and ammonia waste propionic acid ammonium replacement titration etc.Wherein Wu Li just (mensuration---the EDTA-DDTC method of cadmium and Zn content in pigment, chemistry world, 1992,05,223-224) report the method that two-step approach measures cadmium and Zn content in pigment: first with EDTA under mildly acidic conditions sheltering the interference ions measure the total content of cadmium and zinc; Then other a solution total content with EDTA complexometry alkali metal ion, cadmium and zinc under the condition of pH=10 is got, sodium diethyldithiocarbamate (DDTC sodium salt) is used to displace cadmium afterwards, discharge the EDTA of equivalent simultaneously, use magnesium sulfate standard solution titration EDTA again, obtain the content of cadmium, finally calculate the content of zinc with difference assay.The method step is more, and when the content of Te is more than 50% in CZT monocrystalline, can generate the oxide precipitation of white under mild acid conditions, and the observation of interference titration end-point makes terminal variable color insensitive, cannot carry out accurate titration.
Summary of the invention
In view of Problems existing in background technology, the object of the present invention is to provide the method for testing of constant cadmium and zinc in a kind of tellurium-zincium-cadmium crystal, it can simplify experimental procedure, raise the efficiency, reduce analysis cost, be conducive to the observation of titration end-point simultaneously, reduce relative standard deviation.
To achieve these goals, the invention provides the method for testing of constant cadmium and zinc in a kind of tellurium-zincium-cadmium crystal, comprise step:
Step one, get appropriate tellurium-zincium-cadmium crystal sample solution to be measured or get appropriate tellurium-zincium-cadmium crystal solid sample to be measured solution of obtaining after dissolving, adding ammoniacal liquor (1+1) regulates solution ph to neutral, then adds proper ammonia-ammonium chloride buffer solution and regulate solution ph to be 10 and keep stable;
Step 2, adds proper amount of surfactant in solution, then adds appropriate chromium black T indicator, then uses complexing agent EDTA complexometry, makes solution become pure blue from purple, and the volumetric molar concentration of complexing agent EDTA is C
1, consumption is V
1, then cadmium and the total amount of substance n of zinc
cd+Zncalculated by formula (1):
n
Cd+Zn(mol)=V
1(ml)×C
1(mol/L)×10
-3（1）；
Step 3, adds appropriate DDTC sodium salt, makes it fully dissolve, and DDTC sodium salt optionally precipitates cadmium and discharges the EDTA of equivalent, becomes light red with magnesium nitrate solution titration EDTA to solution, and the volumetric molar concentration of magnesium nitrate solution is C
2, consumption is V
2, then the amount of substance n of cadmium
cdcalculated by formula (2):
n
Cd(mol)=V
2(ml)×C
2(mol/L)×10
-3（2），
The then quality m of cadmium
cdcalculated by formula (3):
m
Cd(g)=n
Cd(mol)×112.411(g/mol) （3）；
Step 4, the amount of substance total amount of substance of cadmium and zinc being deducted cadmium according to difference assay obtains the amount of substance n of zinc
zn, be formula (4):
n
Zn(mol)=n
Cd+Zn(mol)-n
Cd(mol) （4）；
The then quality m of zinc
zncalculated by formula (5):
m
Zn(g)=n
Zn(mol)×65.38(g/mol) （5）。
Beneficial effect of the present invention is:
1. the present invention adds surfactant under weak basic condition, inhibits Te to be hydrolyzed the interference brought, makes reaction be able to quantitative calculating, solves the CZT crystal intense hydrolysis difficult problem that causes titration to carry out under mildly acidic conditions.
2. in the present invention surfactant add the sensitivity that simultaneously improve indicator, be conducive to the observation of titration end-point, reduce relative standard deviation, the relative standard deviation of cadmium is no more than 0.2%, the relative standard deviation of zinc is no more than 4.2%, and the recovery of standard addition of cadmium and zinc is 90% ~ 110%.
3. in tellurium-zincium-cadmium crystal of the present invention, the method for testing of constant cadmium and zinc simplifies experimental procedure, improves efficiency, reduces analysis cost.
4. the method for testing of constant cadmium and zinc in tellurium-zincium-cadmium crystal of the present invention, simple to operate and result accurate, can be used for tellurium-zincium-cadmium crystal and other is mainly containing the product quality monitoring of constant tellurium, zinc and cadmium element sample.
Embodiment
The following detailed description of method of testing and the embodiment of constant cadmium and zinc in tellurium-zincium-cadmium crystal according to the present invention.
First method of testing according to constant cadmium and zinc in tellurium-zincium-cadmium crystal of the present invention is described, comprises step:
Step one, get appropriate tellurium-zincium-cadmium crystal sample solution to be measured or get appropriate tellurium-zincium-cadmium crystal solid sample to be measured solution of obtaining after dissolving, adding ammoniacal liquor regulates solution ph to neutral, then adds proper ammonia-ammonium chloride buffer solution and regulate solution ph to be 10 and keep stable;
Step 2, adds proper amount of surfactant in solution, then adds appropriate chromium black T indicator, then uses complexing agent EDTA complexometry, makes solution become pure blue from purple, and the volumetric molar concentration of complexing agent EDTA is C
1, consumption is V
1, then cadmium and the total amount of substance n of zinc
cd+Zncalculated by formula (1):
n
Cd+Zn(mol)=V
1(ml)×C
1(mol/L)×10
-3（1）；
Step 3, adds appropriate DDTC sodium salt, makes it fully dissolve, and DDTC sodium salt optionally precipitates cadmium and discharges the EDTA of equivalent, becomes light red with magnesium nitrate solution titration EDTA to solution, and the volumetric molar concentration of magnesium nitrate solution is C
2, consumption is V
2, then the amount of substance n of cadmium
cdcalculated by formula (2):
n
Cd(mol)=V
2(ml)×C
2(mol/L)×10
-3（2），
The then quality m of cadmium
cdcalculated by formula (3):
m
Cd(g)=n
Cd(mol)×112.411(g/mol) （3）；
Step 4, the amount of substance total amount of substance of cadmium and zinc being deducted cadmium according to difference assay obtains the amount of substance n of zinc
zn, be formula (4):
n
Zn(mol)=n
Cd+Zn(mol)-n
Cd(mol) （4），
The then quality m of zinc
zncalculated by formula (5):
m
Zn(g)=n
Zn(mol)×65.38(g/mol) （5）。
In tellurium-zincium-cadmium crystal according to the present invention constant cadmium and zinc method of testing in, in described step one, tellurium-zincium-cadmium crystal solid sample to be measured can use nitric acid (1+1) to dissolve.
In tellurium-zincium-cadmium crystal according to the present invention constant cadmium and zinc method of testing in, in described step 2, surfactant can be Triton X-100.
In tellurium-zincium-cadmium crystal according to the present invention constant cadmium and zinc method of testing in, in described step 2, the volumetric concentration of Triton X-100 can be 5% ~ 20%, and addition can be 5mL.
In tellurium-zincium-cadmium crystal according to the present invention constant cadmium and zinc method of testing in, in described step 3, the amount of the DDTC sodium salt added can be 1g ~ 2g.
Following explanation is according to the embodiment of the method for testing of constant cadmium and zinc in tellurium-zincium-cadmium crystal of the present invention and test result.
Embodiment 1
The mensuration of constant cadmium and Zn content in standard sample:
(1) the cadmium powder of 1.1364g99.999% is accurately taken, add 20mL nitric acid (1+1) and heating for dissolving in conical flask, accurately take the tellurium powder of 1.3336g99.999%, add 20mL nitric acid (1+1) heating for dissolving in conical flask, accurately take the zinc metal sheet of 0.6538g99.999%, with a small amount of dissolving with hydrochloric acid in conical flask, the zinc solution dissolved is transferred in the volumetric flask of 1L with cooled cadmium solution together with tellurium solution, add 60mL red fuming nitric acid (RFNA) again, be diluted to scale with pure water, lay in the titer as CZT synthesis.
(2) titer of 25mL CZT synthesis is accurately pipetted in 250mL conical flask with transfer pipet, weakly acidic pH is adjusted to ammoniacal liquor (1+1), now produce a large amount of white precipitate, then add the ammoniacal liquor-ammonium chloride buffer solution of 15mL pH=10, keep solution ph to be 10.
(3) in solution, the Triton X-100 surfactant that 5mL volume solubility is 5% is added, now white precipitate disappears, shake up and make it fully dissolve, then add 0.05g chromium black T indicator (being formed through grinding Homogeneous phase mixing by the eriochrome black T solid of 1:100 and NaCl solid), use concentration C
1eDTA standard solution for 0.0203mol/L is titrated to solution and becomes pure blue from purple, reaches titration end-point, the consumption V of record EDTA
1for 24.52mL.
(4) add 2g DDTC sodium salt in the solution after titration, shake makes it dissolve, and now solution is dusty blue, uses concentration C
2magnesium nitrate standard solution for 0.03014mol/L is titrated to solution and becomes light red, reaches titration end-point, the volume V of the magnesium nitrate that record consumes
2for 8.36mL.
Cadmium content and Zn content computation process as follows:
Cadmium and the total amount of substance n of zinc
cd+Zn:
n
Cd+Zn(mol)=24.52×0.0203×10
-3=4.978×10
-4mol，
The amount of substance n of cadmium
cd:
n
Cd(mol)=8.36×0.03014×10
-3=2.520×10
-4mol，
The quality m of cadmium
cd:
m
Cd(g)=2.520×10-
4×112.411=0.02832g，
The amount of substance n of zinc
zn:
n
Zn(mol)=4.978×10
-4mol-2.520×10
-4=2.458×10
-4mol，
The quality m of zinc
zn:
m
Zn(g)=2.458×10
-4×65.38(g/mol)=0.01607g。
Measurement result: cadmium quality is 0.02832g, relative error is 0.32%, and the quality of zinc is 0.01607g, and relative error is 1.68%.
Embodiment 2
The mensuration of cadmium and Zn content in the CZT crystal that our company produces:
(1) 0.5g ~ 0.6g(is accurately taken accurately to 0.0001g) CdZnTe sample is in conical flask, add 10mL nitric acid (1+1), be heated at low temperatures dissolve completely, transfer in the volumetric flask of 250mL after solution cooling, add 10mL nitric acid (1+1), shake up to scale with pure water constant volume.
(2) accurately pipette 25mL sample solution with transfer pipet, by ammoniacal liquor (1+1) adjust ph to close to neutral, now produce a large amount of white precipitate, then add 15mL ammoniacal liquor-ammonium chloride buffer solution, keep solution ph to be 10.
(3) in solution, the Triton X-100 surfactant that 5mL volumetric concentration is 20% is added, now white precipitate disappears, shake up and make it fully dissolve, then add 0.05g chromium black T indicator (being formed through grinding Homogeneous phase mixing by the eriochrome black T solid of 1:100 and NaCl solid), use concentration C
1eDTA standard solution for 0.0203mol/L is titrated to solution and becomes pure blue by purple, reaches titration end-point, the consumption V of record EDTA
1.
(4) add 1g DDTC sodium salt in the solution after titration, shake makes it dissolve, and now solution is dusty blue, uses concentration C
2magnesium nitrate solution for 0.03014moL/L is titrated to solution and becomes light red, reaches titration end-point, the volume V of the magnesium nitrate solution that record consumes
2.
(5) carry out recovery testu, calculate the recovery.
Table 1 provides test parameter and the measurement result of CdZnTe sample in embodiment 2, wherein m
cZTfor taking the quality of CZT crystal prototype, the CZT crystal prototype taken takes from the head of CZT crystal, middle part and afterbody three positions respectively, and respectively carries out three parallel experiments.
Table 2 provides the parameter and the recovery that in embodiment 2, CdZnTe sample mark-on reclaims.
Finally constant cadmium in tellurium-zincium-cadmium crystal and Direct spectrophotometry result are analyzed.
As can be seen from Table 1, in three parallel experiments, the relative standard deviation of cadmium is no more than 0.2%, and the relative standard deviation of zinc is no more than 4.2%.As can be seen from table 2 recovery testu, the recovery of standard addition of cadmium and zinc is between 90% ~ 110%.In tellurium-zincium-cadmium crystal of the present invention, the method for testing of constant cadmium and zinc can simplify experimental procedure, raises the efficiency, and reduces analysis cost, is conducive to the observation of titration end-point simultaneously, reduces relative standard deviation.
Claims (5)
1. the method for testing of constant cadmium and zinc in tellurium-zincium-cadmium crystal, comprises step:
Step one, get appropriate tellurium-zincium-cadmium crystal sample solution to be measured or get appropriate tellurium-zincium-cadmium crystal solid sample to be measured solution of obtaining after dissolving, adding ammoniacal liquor (1+1) regulates solution ph to neutral, then adds proper ammonia-ammonium chloride buffer solution and regulate solution ph to be 10 and keep stable;
Step 2, adds proper amount of surfactant in solution, then adds appropriate chromium black T indicator, then uses complexing agent EDTA complexometry, makes solution become pure blue from purple, and the volumetric molar concentration of complexing agent EDTA is C
1, consumption is V
1, then cadmium and the total amount of substance n of zinc
cd+Zncalculated by formula (1):
n
Cd+Zn(mol)=V
1(ml)×C
1(mol/L)×10
-3（1）；
Step 3, adds appropriate DDTC sodium salt, makes it fully dissolve, and DDTC sodium salt optionally precipitates cadmium and discharges the EDTA of equivalent, becomes light red with magnesium nitrate solution titration EDTA to solution, and the volumetric molar concentration of magnesium nitrate solution is C
2, consumption is V
2, then the amount of substance n of cadmium
cdcalculated by formula (2):
n
Cd(mol)=V
2(ml)×C
2(mol/L)×10
-3（2），
The then quality m of cadmium
cdcalculated by formula (3):
m
Cd(g)=n
Cd(mol)×112.411(g/mol) （3）；
Step 4, the amount of substance total amount of substance of cadmium and zinc being deducted cadmium according to difference assay obtains the amount of substance n of zinc
zn, be formula (4):
n
Zn(mol)=n
Cd+
Zn(mol)-n
Cd(mol) （4），
The then quality m of zinc
zncalculated by formula (5):
m
Zn(g)=n
Zn(mol)×65.38(g/mol) （5）。
2. the method for testing of constant cadmium and zinc in tellurium-zincium-cadmium crystal according to claim 1, is characterized in that, in described step one, tellurium-zincium-cadmium crystal solid sample nitric acid (1+1) to be measured is dissolved.
3. the method for testing of constant cadmium and zinc in tellurium-zincium-cadmium crystal according to claim 1, it is characterized in that, in described step 2, surfactant is Triton X-100.
4. the method for testing of constant cadmium and zinc in tellurium-zincium-cadmium crystal according to claim 3, it is characterized in that, in described step 2, the volumetric concentration of Triton X-100 is 5% ~ 20%, and addition is 5mL.
5. the method for testing of constant cadmium and zinc in tellurium-zincium-cadmium crystal according to claim 1, it is characterized in that, in described step 3, the amount of the DDTC sodium salt added is 1g ~ 2g.
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Cited By (3)
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| CN105891408A (en) * | 2016-04-01 | 2016-08-24 | 中国科学院青海盐湖研究所 | Method for measuring magnesium and zinc content in alloy at same time and application thereof |
| CN109142004A (en) * | 2018-09-21 | 2019-01-04 | 吉林大学 | The detection method of biologically effective state cadmium in a kind of soil |
| CN111748847A (en) * | 2020-06-12 | 2020-10-09 | 中国电子科技集团公司第十一研究所 | Tellurium-zinc-cadmium crystal batching method |
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| CN110907594A (en) * | 2019-11-22 | 2020-03-24 | 西北矿冶研究院 | Chemical analysis method for measuring cadmium in crude cadmium based on increased complexing stability constant |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105891408A (en) * | 2016-04-01 | 2016-08-24 | 中国科学院青海盐湖研究所 | Method for measuring magnesium and zinc content in alloy at same time and application thereof |
| CN109142004A (en) * | 2018-09-21 | 2019-01-04 | 吉林大学 | The detection method of biologically effective state cadmium in a kind of soil |
| CN111748847A (en) * | 2020-06-12 | 2020-10-09 | 中国电子科技集团公司第十一研究所 | Tellurium-zinc-cadmium crystal batching method |
| CN111748847B (en) * | 2020-06-12 | 2021-11-05 | 中国电子科技集团公司第十一研究所 | Tellurium-zinc-cadmium crystal batching method |
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