CN107421947A - A kind of method of arsenic content in measure gold mine - Google Patents
A kind of method of arsenic content in measure gold mine Download PDFInfo
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- CN107421947A CN107421947A CN201710871740.6A CN201710871740A CN107421947A CN 107421947 A CN107421947 A CN 107421947A CN 201710871740 A CN201710871740 A CN 201710871740A CN 107421947 A CN107421947 A CN 107421947A
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- G—PHYSICS
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- 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
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Abstract
The invention belongs to technical field of analytical chemistry, more particularly to a kind of method for determining arsenic content in gold mine, gold ore sample is passed through sodium peroxide and sodium carbonate fusion by this method, water extracts, solution is acidified with sulfuric acid, reduced with KI, be complexed the elements such as lead, tin, zinc with sodium tartrate, then arsenic content is titrated with iodine standard solution;This method instead of arsenic trioxide demarcation using sodium thiosulfate, and experimentation is not related to poisonous and harmful medicine, it is i.e. safe and environmentally friendly, solve the problems, such as in gold mine that arsenic is measured and surely using poisonous and harmful substance pollution environment, also solved because toxic pharmaceuticals can not be carried out by management and control the problem of test analysis;This method degree of accuracy is high, and measurement range is wide, is adapted to the test analysis of batch samples, can be widely applied to gold mine test analysis field.
Description
Technical field
The invention belongs to technical field of analytical chemistry, and in particular to a kind of method for determining arsenic content in gold mine.
Background technology
Arsenic is a kind of poisonous and hazardous element, and it is enriched with nature, in the industrial production the discharge meeting of arsenic-containing waste water
Environment is caused seriously to pollute, particularly in terms of metal smelt, arsenic can corrode steel stove and pipeline, therefore, Accurate Determining ore
In development of the arsenic content to environment and industry it is most important.At present, the common method for determining arsenic in gold mine has:Spectrophotometric
Method, phosphinous acid salt titration and iodimetric titration etc.;Wherein DDTC-Ag salt AAS has obtained in terms of measure analyzes arsenic content
Promote, but this method need to use harmful chloroform reagent, seriously pollute environment, and staff's health is influenceed, survey
It is narrower to determine scope;Phosphinous acid salt titration has used sodium arsenite and arsenic trioxide poisonous reagent in continuous mode, can be right
Environment causes seriously to pollute, and the reagent belongs to easy poison product processed, is newly promulgated according to 2017《The People's Republic of China (PRC) bans taking addictive drugs
Method》Regulation, the reagent are limited the implementation and popularization of this method by control;Due to larger using toxicity in iodimetric titration
Benzene reagent is tested, not only dangerous but also not environmentally, therefore this method is unfavorable for promoting in actual applications;In summary, by
In determining the reagent strip in gold mine used in arsenic content method next safety and environmental issue, have a strong impact on that arsenic contains in gold mine
Measure the application and popularization of setting analysis method.
The content of the invention
In order to overcome above mentioned problem, the invention provides it is a kind of determine gold mine in arsenic content method, this method avoid
The use of poisonous and harmful reagent, it is safe and environmentally friendly, and this method is simple to operate, measurement range is wide, and measurement result is accurate, is adapted to
The test analysis of batch samples, it can be widely applied to the test analysis field of arsenic content in gold mine.
The method of arsenic content, is comprised the following steps that in a kind of measure gold mine:
Step 1: the gold mine that granularity is 0.038~0.074mm is accurately weighed 0.5000 after crushing, drying~
1.0000g samples are put into nickel crucible, are added 4~6g sodium peroxides-sodium carbonate mixed solvent, are stirred;
5~10min is melted Step 2: nickel crucible is placed in the Muffle furnace that temperature is 650~700 DEG C;
Step 3: taking out nickel crucible from Muffle furnace, after placing 10 minutes, whole nickel crucible is put into and fills boiling water
In 250mL beakers, beaker surface plate is then covered, the material in nickel crucible is purged and arrives beaker by heating after boiling 10 minutes with water
In, take out nickel crucible;
Step 4: adding the hydrogenperoxide steam generator that 1~3mL mass fractions are 30% into above-mentioned beaker, boil 10 minutes
Afterwards, room temperature is cooled to, then the material in beaker is transferred in 100mL colorimetric cylinders, scale is diluted with water to, shakes up, is placed clear
Clearly;
Step 5: pipetting the clear liquid after being clarified in the above-mentioned colorimetric cylinders of 25.00ml in 500mL conical flasks, it is diluted with water to
100mL, add 1 drop concentration be 1g/L phenolphthalein indicator, with (1+1) sulfuric acid and solution to it is colourless after amount 5mL;
Step 6: adding the liquor kalii iodide that 2~5mL concentration is 500g/L into conical flask, heating, which is boiled to solution, is in
Untill light yellow, remove, rinsing conical flask outer surface using flowing water is cooled down;
Step 7: adding the EWNN solution that 25mL concentration is 200g/L into conical flask, 120mL is diluted with water to,
Add 3~5mL concentration and be 5g/L starch solution, then sodium thiosulfate standard solution that concentration is 0.01mol/L is added dropwise to indigo plant
Color takes off;
Step 8: with (1+1) ammoniacal liquor and after solution takes on a red color, (1+1) sulfuric acid to red is added dropwise and disappears, after amount 2~3
Drop, solution is set to be cooled to room temperature in acidity;
Step 9: adding 25mL saturated sodium bicarbonate solutions, being titrated to blueness with iodine standard solution occurs being terminal, remembers
Record titration volumes;
Step 10: the blank test of gold ore sample is not added according to step 1 to step 9;
Step 11: the mass fraction of arsenic is calculated as follows:
In formula:
ωAs--- the mass fraction of arsenic, %;
V1--- the volume of titration sample solution consumption iodine standard solution, mL;
V0--- the volume of titration sample blank solution consumption iodine standard solution, mL;
The factor of f --- iodine standard solution, g/mL;
Wherein
MAs--- the molal weight of arsenic, g/mol;
V2--- divide the volume for taking sample solution in colorimetric cylinder, mL;
V3--- the cumulative volume of sample solution, mL in colorimetric cylinder;
M --- weigh the quality g of sample;
--- the concentration of iodine standard solution, mol/L;
Analysis result is represented to 2 significant digits.
Sodium peroxide-sodium carbonate mixed solvent is sodium peroxide and sodium carbonate according to 2 in described step one:1 ratio
Mix.
In described step seven:
The preparation of sodium thiosulfate standard solution:Weigh 2.6g sodium thiosulfate (Na2S2O3﹒ 5H20) the anhydrous carbon of 0.2g, is added
Sour sodium, it is dissolved in 1000mL water, is cooled down after boiling 10min jointly, it is thio for 0.01mol/L that concentration is filtrated to get after placing two weeks
Metabisulfite solution;
The demarcation of sodium thiosulfate standard solution:0.018g is weighed to dry under the conditions of 120 DEG C ± 2 DEG C to the work of constant weight
Primary standard reagent potassium bichromate, it is placed in iodine flask, adds 25mL water, then add 2g KIs and 20mL (1+5) sulfuric acid solution, shakes
It is even, place 10min in dark place;Again plus 150mL temperature is 15 DEG C~20 DEG C of water, is 0.01mol/L sulphur with the concentration prepared
Sodium thiosulfate solution titrates, and adds 4mL concentration to be 5g/L starch solutions during nearly terminal, continues to be titrated to solution and is changed into BG from blueness
Color, while do blank test;
Concentration [c (the Na of sodium thiosulfate standard solution2S2O3)], numerical value is represented with mole every liter (mol/L), as the following formula
Calculate:
In formula:
The quality of m-potassium bichromate, g;
V1The volume of-hypo solution, mL;
V2The volume of-blank test hypo solution, mL;
The molal weight of M-potassium bichromate,
In described step nine:
The preparation of iodine standard solution:The 1.3g crystalline flake of iodine and 3.5g KIs are weighed, is dissolved in 100mL water, is placed in brown bottle,
Place 2 days, be diluted to 1000mL, shake up;
The demarcation of iodine standard solution:The above-mentioned iodine standard solutions prepared of 35.00~40.00mL are measured, are placed in iodine flask
In, add the water that 150mL temperature is 15 DEG C~20 DEG C, it is 0.1mol/L hydrochloric acid to add 5mL concentration, is 0.01mol/L thio with concentration
Sulfuric acid sodium standard solution titrates, and adds 4mL concentration be 5g/L starch solutions during nearly terminal, continues to be titrated to blueness in solution and disappears;
The blank test of consumption iodine is made of water simultaneously:It is 15 DEG C~20 DEG C of water to take 250mL temperature, add 0.05mL~
The iodine standard solution and 4mL concentration that 0.20mL is prepared are 5g/L starch solutions, are 0.01mol/L sodium thiosulfate marks with concentration
Quasi- solution is titrated to solution blueness and disappeared;
The concentration of KI standard liquidNumerical value is represented with mole every liter (mol/L), is calculated as follows:
In formula:
V1The volume of-sodium thiosulfate standard solution, mL;
V2The volume of-blank test sodium thiosulfate standard solution, mL;
c1The concentration of-sodium thiosulfate standard solution, mol/L;
V3The volume of-iodine standard solution, mL;
V4The volume of the iodine standard solution added in-blank test, mL.
Beneficial effects of the present invention:
Gold ore sample passes through sodium peroxide and sodium carbonate fusion, water extraction, and solution is acidified with sulfuric acid, reduced with KI,
The elements such as lead, tin, zinc are complexed with sodium tartrate, then arsenic content is titrated with iodine standard solution;This method uses sodium thiosulfate generation
Arsenic trioxide demarcation has been replaced, and experimentation is not related to poisonous and harmful medicine, i.e., it is safe and environmentally friendly, solve arsenic amount in gold mine
The problem of measure is using poisonous and harmful substance pollution environment, is also solved because toxic pharmaceuticals by management and control can not be carried out test analysis
Problem;This method degree of accuracy is high, and measurement range is wide, is adapted to the test analysis of batch samples, can be widely applied to gold mine survey
Try analysis field.
Embodiment
The invention will be further described with reference to embodiments.
The preparation of sodium thiosulfate standard solution:Weigh 2.6g sodium thiosulfate (Na2S2O3﹒ 5H20) the anhydrous carbon of 0.2g, is added
Sour sodium, it is dissolved in 1000mL water, is cooled down after boiling 10min jointly, it is thio for 0.01mol/L that concentration is filtrated to get after placing two weeks
Metabisulfite solution;
The demarcation of sodium thiosulfate standard solution:0.018g is weighed to dry under the conditions of 120 DEG C ± 2 DEG C to the work of constant weight
Primary standard reagent potassium bichromate, it is placed in iodine flask, adds 25mL water, then add 2g KIs and 20mL (1+5) sulfuric acid solution, shakes
It is even, place 10min in dark place;Again plus 150mL temperature is 15 DEG C~20 DEG C of water, is 0.01mol/L sulphur with the concentration prepared
Sodium thiosulfate solution titrates, and adds 4mL concentration to be 5g/L starch solutions during nearly terminal, continues to be titrated to solution and is changed into BG from blueness
Color, while do blank test;
Concentration [c (the Na of sodium thiosulfate standard solution2S2O3)], numerical value is represented with mole every liter (mol/L), as the following formula
Calculate:
In formula:
The quality of m-potassium bichromate, g;
V1The volume of-hypo solution, mL;
V2The volume of-blank test hypo solution, mL;
The molal weight of M-potassium bichromate,
In described step nine:
The preparation of iodine standard solution:The 1.3g crystalline flake of iodine and 3.5g KIs are weighed, is dissolved in 100mL water, is placed in brown bottle,
Place 2 days, be diluted to 1000mL, shake up;
The demarcation of iodine standard solution:The above-mentioned iodine standard solutions prepared of 35.00~40.00mL are measured, are placed in iodine flask
In, add the water that 150mL temperature is 15 DEG C~20 DEG C, it is 0.1mol/L hydrochloric acid to add 5mL concentration, is 0.01mol/L thio with concentration
Sulfuric acid sodium standard solution titrates, and adds 4mL concentration be 5g/L starch solutions during nearly terminal, continues to be titrated to blueness in solution and disappears;
The blank test of consumption iodine is made of water simultaneously:It is 15 DEG C~20 DEG C of water to take 250mL temperature, add 0.05mL~
The iodine standard solution and 4mL concentration that 0.20mL is prepared are 5g/L starch solutions, are 0.01mol/L sodium thiosulfate marks with concentration
Quasi- solution is titrated to solution blueness and disappeared;
The concentration of KI standard liquidNumerical value is represented with mole every liter (mol/L), is calculated as follows:
In formula:
V1The volume of-sodium thiosulfate standard solution, mL;
V2The volume of-blank test sodium thiosulfate standard solution, mL;
c1The concentration of-sodium thiosulfate standard solution, mol/L;
V3The volume of-iodine standard solution, mL;
V4The volume of the iodine standard solution added in-blank test, mL.
Embodiment 1
The method of arsenic content, is comprised the following steps that in a kind of measure gold mine:
Put Step 1: the gold mine that granularity is 0.038~0.074mm is accurately weighed into 0.5000g samples after crushing, drying
Into nickel crucible, 4g sodium peroxides-sodium carbonate mixed solvent is added, is stirred;
5min is melted Step 2: nickel crucible is placed in the Muffle furnace that temperature is 650 DEG C;
Step 3: taking out nickel crucible from Muffle furnace, after placing 10 minutes, whole nickel crucible is put into and fills 60mL boiling water
250mL beakers in, then cover beaker surface plate, heating boil 10 minutes after with water by the material purging in nickel crucible to another
In one empty beaker, nickel crucible is taken out;
Step 4: the hydrogenperoxide steam generator that 1mL mass fractions are 30% is added into above-mentioned beaker, after boiling 10 minutes,
Room temperature is cooled to, then the material in beaker is transferred in 100mL colorimetric cylinders, scale is diluted with water to, shakes up, places clarification;
Step 5: pipetting the clear liquid after being clarified in the above-mentioned colorimetric cylinders of 25.00ml in 500mL conical flasks, it is diluted with water to
100mL, add 1 drop concentration be 1g/L phenolphthalein indicator, with (1+1) sulfuric acid and solution to it is colourless after amount 5mL;
Step 6: adding the liquor kalii iodide that 2mL concentration is 500g/L into conical flask, heating is boiled to solution in pale yellow
Untill color, remove, rinsing conical flask outer surface using flowing water is cooled down, and is cooled to room temperature;
Step 7: adding the EWNN solution that 25mL concentration is 200g/L into conical flask, 120mL is diluted with water to,
Add 3mL concentration and be 5g/L starch solution, then sodium thiosulfate standard solution to the blueness that concentration is 0.01mol/L is added dropwise and takes off
Go;
Step 8: with (1+1) ammoniacal liquor and after solution takes on a red color, (1+1) sulfuric acid to red is added dropwise and disappears, after the drop of amount 2,
Solution is set to rinse conical flask outer surface in acidity with flowing water and be cooled down, be cooled to room temperature;
Step 9: adding 25mL saturated sodium bicarbonate solutions, being titrated to blueness with iodine standard solution occurs being terminal, remembers
Record titration volumes;
Step 10: the blank test of gold ore sample is not added according to step 1 to step 9;
Step 11: the mass fraction of arsenic is calculated as follows:
In formula:
ωAs--- the mass fraction of arsenic, %;
V1--- the volume of titration sample solution consumption iodine standard solution, mL;
V0--- the volume of titration sample blank solution consumption iodine standard solution, mL;
The factor of f --- iodine standard solution, g/mL;
Wherein
MAs--- the molal weight of arsenic, g/mol;
V2--- divide the volume for taking sample solution in colorimetric cylinder, mL;
V3--- the cumulative volume of sample solution, mL in colorimetric cylinder;
M --- weigh the quality g of sample;
--- the concentration of iodine standard solution, mol/L;
Analysis result is represented to 2 significant digits.
Sodium peroxide-sodium carbonate mixed solvent is sodium peroxide and sodium carbonate according to 2 in described step one:1 ratio
Mix.
Precision Experiment is carried out with Gold Concentrate under Normal Pressure sample and recovery of standard addition is tested, the precision and accuracy of verification method,
It the results are shown in Table 1 and table 2.
The method precision of table 1
Embodiment 2
The method of arsenic content, is comprised the following steps that in a kind of measure gold mine:
Put Step 1: the gold mine that granularity is 0.038~0.074mm is accurately weighed into 1.0000g samples after crushing, drying
Into nickel crucible, 6g sodium peroxides-sodium carbonate mixed solvent is added, is stirred;
10min is melted Step 2: nickel crucible is placed in the Muffle furnace that temperature is 700 DEG C;
Step 3: taking out nickel crucible from Muffle furnace, after placing 10 minutes, whole nickel crucible is put into and fills 60mL boiling water
250mL beakers in, then cover beaker surface plate, heating boil 10 minutes after with water by the material purging in nickel crucible to another
In one empty beaker, nickel crucible is taken out;
Step 4: the hydrogenperoxide steam generator that 3mL mass fractions are 30% is added into above-mentioned beaker, after boiling 10 minutes,
Room temperature is cooled to, then the material in beaker is transferred in 100mL colorimetric cylinders, scale is diluted with water to, shakes up, places clarification;
Step 5: pipetting the clear liquid after being clarified in the above-mentioned colorimetric cylinders of 25.00ml in 500mL conical flasks, it is diluted with water to
100mL, add 1 drop concentration be 1g/L phenolphthalein indicator, with (1+1) sulfuric acid and solution to it is colourless after amount 5mL;
Step 6: adding the liquor kalii iodide that 5mL concentration is 500g/L into conical flask, heating is boiled to solution in pale yellow
Untill color, remove, rinsing conical flask outer surface using flowing water is cooled down, and is cooled to room temperature;
Step 7: adding the EWNN solution that 25mL concentration is 200g/L into conical flask, 120mL is diluted with water to,
Add 5mL concentration and be 5g/L starch solution, then sodium thiosulfate standard solution to the blueness that concentration is 0.01mol/L is added dropwise and takes off
Go;
Step 8: with (1+1) ammoniacal liquor and after solution takes on a red color, (1+1) sulfuric acid to red is added dropwise and disappears, after the drop of amount 3,
Solution is set to be cooled to room temperature in acidity;
Step 9: adding 25mL saturated sodium bicarbonate solutions, being titrated to blueness with iodine standard solution occurs being terminal, remembers
Record titration volumes;
Step 10: the blank test of gold ore sample is not added according to step 1 to step 9;
Step 11: the mass fraction of arsenic is calculated as follows:
In formula:
ωAs--- the mass fraction of arsenic, %;
V1--- the volume of titration sample solution consumption iodine standard solution, mL;
V0--- the volume of titration sample blank solution consumption iodine standard solution, mL;
The factor of f --- iodine standard solution, g/mL;Wherein
MAs--- the molal weight of arsenic, g/mol;
V2--- divide the volume for taking sample solution in colorimetric cylinder, mL;
V3--- the cumulative volume of sample solution, mL in colorimetric cylinder;
M --- weigh the quality g of sample;
--- the concentration of iodine standard solution, mol/L;
Analysis result is represented to 2 significant digits.
Sodium peroxide-sodium carbonate mixed solvent is sodium peroxide and sodium carbonate according to 2 in described step one:1 ratio
Mix.
Precision Experiment and recovery of standard addition experiment, verification method precision and accuracy are carried out using gold ore sample,
It the results are shown in Table 3 and table 4.
The precision of the method for table 3
Recovery of standard addition is calculated according to below equation:
Recovery of standard addition=(mark-on Specimen Determination value-sample measurements) ÷ mark-on amount × 100%
The recovery of standard addition of the method for table 4
Claims (4)
1. a kind of method for determining arsenic content in gold mine, is comprised the following steps that:
Step 1: the gold mine that granularity is 0.038~0.074mm is accurately weighed into 0.5000~1.0000g samples after crushing, drying
Product are put into nickel crucible, are added 4~6g sodium peroxides-sodium carbonate mixed solvent, are stirred;
5~10min is melted Step 2: nickel crucible is placed in the Muffle furnace that temperature is 650~700 DEG C;
Step 3: taking out nickel crucible from Muffle furnace, after placing 10 minutes, whole nickel crucible is put into the 250mL for filling boiling water
In beaker, beaker surface plate is then covered, the material in nickel crucible is purged into beaker, taken by heating after boiling 10 minutes with water
Go out nickel crucible;
Step 4: the hydrogenperoxide steam generator that 1~3mL mass fractions are 30% is added into above-mentioned beaker, it is cold after boiling 10 minutes
But to room temperature, then the material in beaker is transferred in 100mL colorimetric cylinders, is diluted with water to scale, shakes up, place clarification;
Step 5: pipetting the clear liquid after being clarified in the above-mentioned colorimetric cylinders of 25.00ml in 500mL conical flasks, it is diluted with water to
100mL, add 1 drop concentration be 1g/L phenolphthalein indicator, with (1+1) sulfuric acid and solution to it is colourless after amount 5mL;
Step 6: adding the liquor kalii iodide that 2~5mL concentration is 500g/L into conical flask, heating is boiled to solution in pale yellow
Untill color, remove, be cooled to room temperature;
Step 7: adding the EWNN solution that 25mL concentration is 200g/L into conical flask, 120mL is diluted with water to, adds 3
~5mL concentration is 5g/L starch solution, then sodium thiosulfate standard solution to the blueness that concentration is 0.01mol/L is added dropwise and takes off
Go;
Step 8: with (1+1) ammoniacal liquor and after solution takes on a red color, (1+1) sulfuric acid to red is added dropwise and disappears, after the drop of amount 2~3,
Solution is set to be cooled to room temperature in acidity;
Step 9: adding 25mL saturated sodium bicarbonate solutions, being titrated to blueness with iodine standard solution occurs being terminal, records drop
Determine volume;
Step 10: the blank test of gold ore sample is not added according to step 1 to step 9;
Step 11: the mass fraction of arsenic is calculated as follows:
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In formula:
ωAs--- the mass fraction of arsenic, %;
V1--- the volume of titration sample solution consumption iodine standard solution, mL;
V0--- the volume of titration sample blank solution consumption iodine standard solution, mL;
The factor of f --- iodine standard solution, g/mL;
Wherein
MAs--- the molal weight of arsenic, g/mol;
V2--- divide the volume for taking sample solution in colorimetric cylinder, mL;
V3--- the cumulative volume of sample solution, mL in colorimetric cylinder;
M --- weigh the quality g of sample;
--- the concentration of iodine standard solution, mol/L;
Analysis result is represented to 2 significant digits.
2. a kind of method for determining arsenic content in gold mine according to claim 1, it is characterised in that in described step one
Sodium peroxide-sodium carbonate mixed solvent is sodium peroxide and sodium carbonate according to 2:1 ratio mixes.
3. a kind of method for determining arsenic content in gold mine according to claim 2, it is characterised in that in described step seven:
The preparation of sodium thiosulfate standard solution:Weigh 2.6g sodium thiosulfate (Na2S2O3﹒ 5H20) 0.2g natrium carbonicum calcinatums, are added,
It is dissolved in 1000mL water, is cooled down after boiling 10min jointly, it is 0.01mol/L thiosulfuric acids to be filtrated to get concentration after placing two weeks
Sodium solution;
The demarcation of sodium thiosulfate standard solution:0.018g is weighed to dry under the conditions of 120 DEG C ± 2 DEG C to the working standard of constant weight
Reagent potassium bichromate, is placed in iodine flask, adds 25mL water, then adds 2g KIs and 20mL (1+5) sulfuric acid solution, shakes up, in
Place 10min in dark place;Again plus 150mL temperature is 15 DEG C~20 DEG C of water, is 0.01mol/L thiosulfuric acids with the concentration prepared
Sodium solution titrates, and adds 4mL concentration to be 5g/L starch solutions during nearly terminal, continues to be titrated to solution and is changed into bright green from blueness, together
When do blank test;
Concentration [c (the Na of sodium thiosulfate standard solution2S2O3)], numerical value is represented with mole every liter (mol/L), is calculated as follows:
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In formula:
The quality of m-potassium bichromate, g;
V1The volume of-hypo solution, mL;
V2The volume of-blank test hypo solution, mL;
The molal weight of M-potassium bichromate,
4. a kind of method for determining arsenic content in gold mine according to claim 3, it is characterised in that in described step nine:
The preparation of iodine standard solution:The 1.3g crystalline flake of iodine and 3.5g KIs are weighed, is dissolved in 100mL water, is placed in brown bottle, is placed
2 days, 1000mL is diluted to, is shaken up;
The demarcation of iodine standard solution:The above-mentioned iodine standard solutions prepared of 35.00~40.00mL are measured, is placed in iodine flask, adds
150mL temperature is 15 DEG C~20 DEG C of water, and it is 0.1mol/L hydrochloric acid to add 5mL concentration, is 0.01mol/L sodium thiosulfate with concentration
Standard liquid titrates, and adds 4mL concentration be 5g/L starch solutions during nearly terminal, continues to be titrated to blueness in solution and disappears;
The blank test of consumption iodine is made of water simultaneously:The water that 250mL temperature is 15 DEG C~20 DEG C is taken, adds 0.05mL~0.20mL
The iodine standard solution and 4mL concentration prepared is 5g/L starch solutions, is 0.01mol/L sodium thiosulfate standard solutions with concentration
Solution blueness is titrated to disappear;
The concentration of KI standard liquidNumerical value is represented with mole every liter (mol/L), is calculated as follows:
<mrow>
<mi>c</mi>
<mrow>
<mo>(</mo>
<mfrac>
<mn>1</mn>
<mn>2</mn>
</mfrac>
<msub>
<mi>I</mi>
<mn>2</mn>
</msub>
<mo>)</mo>
</mrow>
<mo>=</mo>
<mfrac>
<mrow>
<mo>(</mo>
<msub>
<mi>V</mi>
<mn>1</mn>
</msub>
<mo>-</mo>
<msub>
<mi>V</mi>
<mn>2</mn>
</msub>
<mo>)</mo>
<mo>&times;</mo>
<msub>
<mi>c</mi>
<mn>1</mn>
</msub>
</mrow>
<mrow>
<msub>
<mi>V</mi>
<mn>3</mn>
</msub>
<mo>-</mo>
<msub>
<mi>V</mi>
<mn>4</mn>
</msub>
</mrow>
</mfrac>
</mrow>
In formula:
V1The volume of-sodium thiosulfate standard solution, mL;
V2The volume of-blank test sodium thiosulfate standard solution, mL;
c1The concentration of-sodium thiosulfate standard solution, mol/L;
V3The volume of-iodine standard solution, mL;
V4The volume of the iodine standard solution added in-blank test, mL.
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CN108318481A (en) * | 2017-12-26 | 2018-07-24 | 漳州傲农牧业科技有限公司 | The detection method of Absorbance ratio-derivative method in a kind of montmorillonite |
CN108444931A (en) * | 2018-02-13 | 2018-08-24 | 长春黄金研究院有限公司 | A kind of method of arsenic content in measurement gold mine |
CN109142618A (en) * | 2018-09-10 | 2019-01-04 | 江西铜业股份有限公司 | A kind of method of trivalent arsenic in quick measurement acidic arsenic-containing liquid |
CN110836947A (en) * | 2018-08-15 | 2020-02-25 | 青岛海湾精细化工有限公司 | Method for detecting active ingredients of pyrazolone |
CN113759072A (en) * | 2021-09-02 | 2021-12-07 | 中铝洛阳铜加工有限公司 | Method for measuring arsenic content in copper-arsenic intermediate alloy |
CN117310079A (en) * | 2023-11-30 | 2023-12-29 | 长春黄金研究院有限公司 | Method for continuously measuring arsenic and copper in arsenic-containing gold concentrate |
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CN108444931A (en) * | 2018-02-13 | 2018-08-24 | 长春黄金研究院有限公司 | A kind of method of arsenic content in measurement gold mine |
CN110836947A (en) * | 2018-08-15 | 2020-02-25 | 青岛海湾精细化工有限公司 | Method for detecting active ingredients of pyrazolone |
CN109142618A (en) * | 2018-09-10 | 2019-01-04 | 江西铜业股份有限公司 | A kind of method of trivalent arsenic in quick measurement acidic arsenic-containing liquid |
CN109142618B (en) * | 2018-09-10 | 2021-07-16 | 江西铜业股份有限公司 | Method for rapidly determining trivalent arsenic in acidic arsenic-containing liquid |
CN113759072A (en) * | 2021-09-02 | 2021-12-07 | 中铝洛阳铜加工有限公司 | Method for measuring arsenic content in copper-arsenic intermediate alloy |
CN117310079A (en) * | 2023-11-30 | 2023-12-29 | 长春黄金研究院有限公司 | Method for continuously measuring arsenic and copper in arsenic-containing gold concentrate |
CN117310079B (en) * | 2023-11-30 | 2024-01-30 | 长春黄金研究院有限公司 | Method for continuously measuring arsenic and copper in arsenic-containing gold concentrate |
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