CN105445412A - Method for determining copper content in copper telluride - Google Patents

Method for determining copper content in copper telluride Download PDF

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CN105445412A
CN105445412A CN201510797488.XA CN201510797488A CN105445412A CN 105445412 A CN105445412 A CN 105445412A CN 201510797488 A CN201510797488 A CN 201510797488A CN 105445412 A CN105445412 A CN 105445412A
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copper
sample
solution
add
sodium thiosulfate
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CN105445412B (en
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展之旺
余江鸿
王同敏
王红燕
方彦霞
路军兵
张彦翠
齐白羽
赵海军
郑省政
张晨洁
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Northwest Research Institute of Mining and Metallurgy
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
    • G01N31/166—Continuous titration of flowing liquids

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Abstract

The invention belongs to the technical field of chemical analysis, and relates to a method for determining copper content in copper telluride. In the invention, hydrobromic acid is used As a volatile reagent to form volatile bromide to Se, Sn, As and other impurity ions in copper telluride for heating and volatilization in a sample pretreatment stage, so that inaccurate results caused by selenium oxidizing potassium iodide and arsenic reducing iodine are avoided; meanwhile, concentrated sulfuric acid is used for smoking and evaporating the sample to dryness so as to ensure that no + 4-valent tellurium exists, ensure that tellurium does not participate in the reaction, and ensure the reliability and accuracy of the result.

Description

A kind of method measuring copper content in telluride copper
Technical field
The invention belongs to chemical analysis technology field, relate to a kind of method measuring copper content in telluride copper.
Background technology
Telluride copper is the crystal powder of black, more stable in atmosphere under normal temperature.Telluride copper is not only important inorganic material, or stores the fabulous form of tellurium and copper resource.In sulfuric acid solution, replace Te with Cu and generate telluride copper, make tellurium and many separation of metal ions and obtain quite high enrichment.Cu replaces Te, can be+4 valencys or+6 valencys, all can generate Cu2Te, namely not affect by the valence state of tellurium. in the presence of an oxidizer telluride copper can with acid or alkali generation chemical reaction, this is also be separated and reclaim the foundation of Cu and Te.In a word, tellurium and copper mutual chemical combination and to reclaim tellurium from solution be very distinctive at relatively high temperatures.
Often use iodimetric titration to carry out for copper content testing in telluride copper, the acidity of iodimetric titration reaction is pH=3.5 ~ 4; When acidity is excessive, the easy oxidation by air of iodide and separate out iodine, also can increase the solubleness of cuprous iodide simultaneously, and as pH>4, the hypoiodite of iodine formation extremely unstable, itself has redox reaction, can be analyzed to: 2OH ~+ I 2→ I ~+ IO ~+ H 2o, 3IO ~→ 2I ~+ IO 3 ~, IO in the acid solution of titration 3 ~and I ~point parsing iodine, making terminal unstable.
Summary of the invention
The object of the invention is to provide a kind of method measuring copper content in telluride copper for prior art Problems existing.
Measure a method for copper content in telluride copper, it is characterized in that, comprise the following steps:
(1) sodium thiosulfate standard solution is demarcated: the actual concentrations cmol/L measuring sodium thiosulfate volumetric soiutions;
(2) pre-service telluride copper sample to be tested: take quality m 0the telluride copper sample to be tested of=0.2000 ~ 0.5000g is placed in beaker, adds 5 ~ 15mL nitric acid in beaker, and heating makes telluride copper sample to be tested dissolve completely, then in beaker, add 8 ~ 20mL sulfuric acid (1+1), is heated to emit dense white cigarette, cooling; In beaker, add 10 ~ 15 your mL hydrobromic acids, be slowly heated to emit dense white cigarette, cooling; In beaker, add 3 ~ 5mL sulfuric acid (1+1) and 10 ~ 15mL hydrobromic acid, be again slowly heated to white cigarette and emit to the greatest extent, cooling;
(3) mensuration of copper content in sample: drip hydrochloric acid in pretreated telluride copper sample to be tested, boil and solubility salt is dissolved completely, be cooled to room temperature; Ammonium acetate solution to the redness in sample dripping concentration 300g/L is no longer deepened and excessive 3 ~ 5mL, then drips red in ammonium bifluoride saturated solution to sample disappearance and excessive 1mL, mixing; Add 2 ~ 3g potassium iodide, shake is dissolved, be titrated to light yellow immediately with sodium thiosulfate standard solution, add the starch solution 2mL of concentration 5g/L, continue to be titrated to sodium thiosulfate standard solution light blue, add the potassium thiocyanate solution 5mL of concentration 100g/L, commove to blueness and deepen, sodium thiosulfate standard solution continues to be titrated to blueness and just disappears for terminal, records the volume V of the hypo solution consumed 3mL; Blank test is done, the volume V of the hypo solution that record blank solution consumes in company with sample 2mL;
(4) numerical value in above-mentioned steps is brought into the content ω of copper in following formulae discovery telluride copper sample cu%:
；
In formula, for the molal weight of copper.
The present invention has following beneficial effect:
The present invention the sample pretreatment stage adopt hydrobromic acid as be vaporized reagent to telluride copper in the foreign ion such as Se, Sn, As form volatile bromide and carry out heating volatilization, thus avoid selenolite potassium iodide, arsenic reduces iodine and causes result inaccurate; Smolder evaporate to dryness sample to ensure there are not+4 valency telluriums with the concentrated sulphuric acid simultaneously, guarantees that tellurium does not participate in reaction, ensure that reliability and the accuracy of result.
Embodiment
Embodiment 1
Measure a method for copper content in telluride copper, comprise the following steps:
(1) sodium thiosulfate standard solution is demarcated: take quality m=0.070g fine copper three parts, be placed in 500mL conical beaker, slowly add 10mL nitric acid, cover table ware, be placed in electric hot plate low temperature to go out, heating makes it dissolve completely, adds 5mL sulfuric acid (1+1), continue heating to steam to dry to the greatest extent, take off slightly cold; With 40mL water purge wall of cup, heating is boiled and salt is dissolved completely, takes off and is chilled to room temperature; Add 1mL glacial acetic acid (1+3), add 3mL ammonium bifluoride saturated solution, shake up; Add 2g ~ 3g potassium iodide, shake is dissolved, be titrated to light yellow immediately with sodium thiosulfate standard solution, add the starch solution 2mL of concentration 5g/L, continue to be titrated to sodium thiosulfate standard solution light blue, add the potassium thiocyanate solution 5mL of concentration 100g/L, commove to blueness and deepen, being titrated to that blueness just disappears with sodium thiosulfate standard solution is terminal, records the volume V of the hypo solution consumed 1mL; Doing blank test in company with demarcating, recording the volume V of the hypo solution consumed 0;
Numerical value in above-mentioned steps is brought into the concentration c mol/L of following formulae discovery sodium thiosulfate volumetric soiutions:
,
In formula, for the molal weight of copper;
Carry out three parallel experiments, choosing mean value is sodium thiosulfate volumetric soiutions actual concentrations, and the consumption of sodium thiosulfate and measured value are in table 1;
；
(2) pre-service telluride copper sample to be tested: take quality m 0the telluride copper sample to be tested of=0.5000g is placed in beaker, adds 15mL nitric acid in beaker, and heating makes telluride copper sample to be tested dissolve completely, then in beaker, add 20mL sulfuric acid (1+1), is heated to emit dense white cigarette, cooling; In beaker, add 15mL hydrobromic acid, be slowly heated to emit dense white cigarette, cooling; In beaker, add 5mL sulfuric acid (1+1) and 15mL hydrobromic acid, be again slowly heated to white cigarette and emit to the greatest extent, cooling;
(3) mensuration of copper content in sample: drip hydrochloric acid in pretreated telluride copper sample to be tested, boil and solubility salt is dissolved completely, be cooled to room temperature; Ammonium acetate solution to the redness in sample dripping concentration 300g/L is no longer deepened and excessive 3 ~ 5mL, then drips red in ammonium bifluoride saturated solution to sample disappearance and excessive 1mL, mixing; Add 2 ~ 3g potassium iodide, shake is dissolved, be titrated to light yellow immediately with sodium thiosulfate standard solution, add the starch solution 2mL of concentration 5g/L, continue to be titrated to sodium thiosulfate standard solution light blue, add the potassium thiocyanate solution 5mL of concentration 100g/L, commove to blueness and deepen, sodium thiosulfate standard solution continues to be titrated to blueness and just disappears for terminal, records the volume V of the hypo solution consumed 3mL; Blank test is done, the volume V of the hypo solution that record blank solution consumes in company with sample 2mL;
(4) numerical value in above-mentioned steps is brought into the content ω of copper in following formulae discovery telluride copper sample cu%:
,
In formula, for the molal weight of copper;
Carry out three parallel experiments, choose the content that mean value is copper in telluride copper sample, reagent dosage and style measured value are in table 2;
。
Embodiment 2
Measure a method for copper content in telluride copper, comprise the following steps:
(1) sodium thiosulfate standard solution is demarcated: take quality m=0.070g fine copper three parts, be placed in 500mL conical beaker, slowly add 10mL nitric acid, cover table ware, be placed in electric hot plate low temperature to go out, heating makes it dissolve completely, adds 5mL sulfuric acid (1+1), continue heating to steam to dry to the greatest extent, take off slightly cold; With 40mL water purge wall of cup, heating is boiled and salt is dissolved completely, takes off and is chilled to room temperature; Add 1mL glacial acetic acid (1+3), add 3mL ammonium bifluoride saturated solution, shake up; Add 2g ~ 3g potassium iodide, shake is dissolved, be titrated to light yellow immediately with sodium thiosulfate standard solution, add the starch solution 2mL of concentration 5g/L, continue to be titrated to sodium thiosulfate standard solution light blue, add the potassium thiocyanate solution 5mL of concentration 100g/L, commove to blueness and deepen, being titrated to that blueness just disappears with sodium thiosulfate standard solution is terminal, records the volume V of the hypo solution consumed 1mL; Doing blank test in company with demarcating, recording the volume V of the hypo solution consumed 0;
Numerical value in above-mentioned steps is brought into the concentration c mol/L of following formulae discovery sodium thiosulfate volumetric soiutions:
’
In formula, for the molal weight of copper;
Carry out three parallel experiments, choosing mean value is sodium thiosulfate volumetric soiutions actual concentrations, and the consumption of sodium thiosulfate and measured value are in table 3;
，
(2) pre-service telluride copper sample to be tested: take quality m 0the telluride copper sample to be tested of=0.2000g is placed in beaker, adds 5mL nitric acid in beaker, and heating makes telluride copper sample to be tested dissolve completely, then in beaker, add 8mL sulfuric acid (1+1), is heated to emit dense white cigarette, cooling; In beaker, add 10mL hydrobromic acid, be slowly heated to emit dense white cigarette, cooling; In beaker, add 3mL sulfuric acid (1+1) and 10mL hydrobromic acid, be again slowly heated to white cigarette and emit to the greatest extent, cooling;
(3) mensuration of copper content in sample: drip hydrochloric acid in pretreated telluride copper sample to be tested, boil and solubility salt is dissolved completely, be cooled to room temperature; Ammonium acetate solution to the redness in sample dripping concentration 300g/L is no longer deepened and excessive 3 ~ 5mL, then drips red in ammonium bifluoride saturated solution to sample disappearance and excessive 1mL, mixing; Add 2 ~ 3g potassium iodide, shake is dissolved, be titrated to light yellow immediately with sodium thiosulfate standard solution, add the starch solution 2mL of concentration 5g/L, continue to be titrated to sodium thiosulfate standard solution light blue, add the potassium thiocyanate solution 5mL of concentration 100g/L, commove to blueness and deepen, sodium thiosulfate standard solution continues to be titrated to blueness and just disappears for terminal, records the volume V of the hypo solution consumed 3mL; Blank test is done, the volume V of the hypo solution that record blank solution consumes in company with sample 2mL;
(4) numerical value in above-mentioned steps is brought into the content ω of copper in following formulae discovery telluride copper sample cu%:
,
In formula, for the molal weight of copper;
Carry out three parallel experiments, choose the content that mean value is copper in telluride copper sample, reagent dosage and style measured value are in table 4;
。
Embodiment 3
Measure a method for copper content in telluride copper, comprise the following steps:
(1) sodium thiosulfate standard solution is demarcated: take quality m=0.070g fine copper three parts, be placed in 500mL conical beaker, slowly add 10mL nitric acid, cover table ware, be placed in electric hot plate low temperature to go out, heating makes it dissolve completely, adds 5mL sulfuric acid (1+1), continue heating to steam to dry to the greatest extent, take off slightly cold; With 40mL water purge wall of cup, heating is boiled and salt is dissolved completely, takes off and is chilled to room temperature; Add 1mL glacial acetic acid (1+3), add 3mL ammonium bifluoride saturated solution, shake up; Add 2g ~ 3g potassium iodide, shake is dissolved, be titrated to light yellow immediately with sodium thiosulfate standard solution, add the starch solution 2mL of concentration 5g/L, continue to be titrated to sodium thiosulfate standard solution light blue, add the potassium thiocyanate solution 5mL of concentration 100g/L, commove to blueness and deepen, being titrated to that blueness just disappears with sodium thiosulfate standard solution is terminal, records the volume V of the hypo solution consumed 1mL; Doing blank test in company with demarcating, recording the volume V of the hypo solution consumed 0;
Numerical value in above-mentioned steps is brought into the concentration c mol/L of following formulae discovery sodium thiosulfate volumetric soiutions:
,
In formula, for the molal weight of copper;
Carry out three parallel experiments, choosing mean value is sodium thiosulfate volumetric soiutions actual concentrations, and the consumption of sodium thiosulfate and measured value are in table 5;
；
(2) pre-service telluride copper sample to be tested: take quality m 0the telluride copper sample to be tested of=0.3000g is placed in beaker, adds 10mL nitric acid in beaker, and heating makes telluride copper sample to be tested dissolve completely, then in beaker, add 10mL sulfuric acid (1+1), is heated to emit dense white cigarette, cooling; In beaker, add 10mL hydrobromic acid, be slowly heated to emit dense white cigarette, cooling; In beaker, add 3mL sulfuric acid (1+1) and 10mL hydrobromic acid, be again slowly heated to white cigarette and emit to the greatest extent, cooling;
(3) mensuration of copper content in sample: drip hydrochloric acid in pretreated telluride copper sample to be tested, boil and solubility salt is dissolved completely, be cooled to room temperature; Ammonium acetate solution to the redness in sample dripping concentration 300g/L is no longer deepened and excessive 3 ~ 5mL, then drips red in ammonium bifluoride saturated solution to sample disappearance and excessive 1mL, mixing; Add 2 ~ 3g potassium iodide, shake is dissolved, be titrated to light yellow immediately with sodium thiosulfate standard solution, add the starch solution 2mL of concentration 5g/L, continue to be titrated to sodium thiosulfate standard solution light blue, add the potassium thiocyanate solution 5mL of concentration 100g/L, commove to blueness and deepen, sodium thiosulfate standard solution continues to be titrated to blueness and just disappears for terminal, records the volume V of the hypo solution consumed 3mL; Blank test is done, the volume V of the hypo solution that record blank solution consumes in company with sample 2mL;
(4) numerical value in above-mentioned steps is brought into the content ω of copper in following formulae discovery telluride copper sample cu%:
,
In formula, for the molal weight of copper;
Carry out three parallel experiments, choose the content that mean value is copper in telluride copper sample, reagent dosage and style measured value are in table 6;
。
Embodiment 4
Measure a method for copper content in telluride copper, comprise the following steps:
(1) sodium thiosulfate standard solution is demarcated: take quality m=0.070g fine copper three parts, be placed in 500mL conical beaker, slowly add 10mL nitric acid, cover table ware, be placed in electric hot plate low temperature to go out, heating makes it dissolve completely, adds 5mL sulfuric acid (1+1), continue heating to steam to dry to the greatest extent, take off slightly cold; With 40mL water purge wall of cup, heating is boiled and salt is dissolved completely, takes off and is chilled to room temperature; Add 1mL glacial acetic acid (1+3), add 3mL ammonium bifluoride saturated solution, shake up; Add 2g ~ 3g potassium iodide, shake is dissolved, be titrated to light yellow immediately with sodium thiosulfate standard solution, add the starch solution 2mL of concentration 5g/L, continue to be titrated to sodium thiosulfate standard solution light blue, add the potassium thiocyanate solution 5mL of concentration 100g/L, commove to blueness and deepen, being titrated to that blueness just disappears with sodium thiosulfate standard solution is terminal, records the volume V of the hypo solution consumed 1mL; Doing blank test in company with demarcating, recording the volume V of the hypo solution consumed 0;
Numerical value in above-mentioned steps is brought into the concentration c mol/L of following formulae discovery sodium thiosulfate volumetric soiutions:
’
In formula, for the molal weight of copper;
Carry out three parallel experiments, choosing mean value is sodium thiosulfate volumetric soiutions actual concentrations, and the consumption of sodium thiosulfate and measured value are in table 7;
；
(2) pre-service telluride copper sample to be tested: take quality m 0the telluride copper sample to be tested of=0.4000g is placed in beaker, adds 15mL nitric acid in beaker, and heating makes telluride copper sample to be tested dissolve completely, then in beaker, add 15mL sulfuric acid (1+1), is heated to emit dense white cigarette, cooling; In beaker, add 10mL hydrobromic acid, be slowly heated to emit dense white cigarette, cooling; In beaker, add 5mL sulfuric acid (1+1) and 10mL hydrobromic acid, be again slowly heated to white cigarette and emit to the greatest extent, cooling.
(3) mensuration of copper content in sample: drip hydrochloric acid in pretreated telluride copper sample to be tested, boil and solubility salt is dissolved completely, be cooled to room temperature; Ammonium acetate solution to the redness in sample dripping concentration 300g/L is no longer deepened and excessive 3 ~ 5mL, then drips red in ammonium bifluoride saturated solution to sample disappearance and excessive 1mL, mixing; Add 2 ~ 3g potassium iodide, shake is dissolved, be titrated to light yellow immediately with sodium thiosulfate standard solution, add the starch solution 2mL of concentration 5g/L, continue to be titrated to sodium thiosulfate standard solution light blue, add the potassium thiocyanate solution 5mL of concentration 100g/L, commove to blueness and deepen, sodium thiosulfate standard solution continues to be titrated to blueness and just disappears for terminal, records the volume V of the hypo solution consumed 3mL; Blank test is done, the volume V of the hypo solution that record blank solution consumes in company with sample 2mL.
(4) numerical value in above-mentioned steps is brought into the content ω of copper in following formulae discovery telluride copper sample cu%:
,
In formula, for the molal weight of copper;
Carry out three parallel experiments, choose the content that mean value is copper in telluride copper sample, reagent dosage and style measured value are in table 8;
。

Claims (1)

1. measure a method for copper content in telluride copper, it is characterized in that, comprise the following steps:
(1) demarcate sodium thiosulfate standard solution, measure the actual concentrations cmol/L of sodium thiosulfate volumetric soiutions;
(2) pre-service telluride copper sample to be tested: take quality m 0the telluride copper sample to be tested of=0.2000 ~ 0.5000g is placed in beaker, adds 5 ~ 15mL nitric acid in beaker, and heating makes telluride copper sample to be tested dissolve completely, then in beaker, add 8 ~ 20mL sulfuric acid (1+1), is heated to emit dense white cigarette, cooling; In beaker, add 10 ~ 15mL hydrobromic acid, be slowly heated to emit dense white cigarette, cooling; In beaker, add 3 ~ 5mL sulfuric acid (1+1) and 10 ~ 15mL hydrobromic acid, be again slowly heated to white cigarette and emit to the greatest extent, cooling;
(3) mensuration of copper content in sample: drip hydrochloric acid in pretreated telluride copper sample to be tested, boil and solubility salt is dissolved completely, be cooled to room temperature; Ammonium acetate solution to the redness in sample dripping concentration 300g/L is no longer deepened and excessive 3 ~ 5mL, then drips red in ammonium bifluoride saturated solution to sample disappearance and excessive 1mL, mixing; Add 2 ~ 3g potassium iodide, shake is dissolved, be titrated to light yellow immediately with sodium thiosulfate standard solution, add the starch solution 2mL of concentration 5g/L, continue to be titrated to sodium thiosulfate standard solution light blue, add the potassium thiocyanate solution 5mL of concentration 100g/L, commove to blueness and deepen, sodium thiosulfate standard solution continues to be titrated to blueness and just disappears for terminal, records the volume V of the hypo solution consumed 3mL; Blank test is done, the volume V of the hypo solution that record blank solution consumes in company with sample 2mL;
(4) numerical value in above-mentioned steps is brought into the content ω of copper in following formulae discovery telluride copper sample cu%:
；
In formula, M is the molal weight of copper.
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Publication number Priority date Publication date Assignee Title
CN112798733A (en) * 2021-04-14 2021-05-14 北矿检测技术有限公司 Method for detecting copper content in waste magnesia brick and application

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