CN108680562A - The assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings - Google Patents
The assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings Download PDFInfo
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Abstract
The present invention relates to a kind of assay methods of copper-lead zinc-manganese cadmium chromium in cyaniding tail washings, belong to the assay method of metal in cyaniding tail washings.Cyaniding tail washings is taken to be placed in conical flask, potassium chlorate is added, ammonium acid fluoride, sample connects hydrocyanic acid absorption plant, nitric acid is added, after sample digestion, perchloric acid and sulfuric acid is added, then it steams to dipping dry, slightly cold rear each tenor that salt Ore Leaching is added, carries out in analysis measurement cyaniding tail washings to standard solution, blank and sample with inductive coupling plasma emission spectrum.The analysis method of the present invention is effective, it is accurate quickly, while it is easy to operate, it can be achieved that sample batch operation, the real-time monitoring to the heavy metal ion content in cyaniding tail washings, the recycling of valuable metal, the sustainable development important in inhibiting of environment.
Description
Technical field
The present invention relates to the assay methods of copper, lead, zinc, manganese, cadmium, chromium in gold industry cyanidation technology tail washings.
Background technology
In the evolution of golden production, cyaniding is as one of methods of noble metals such as most effective extraction gold and silver, more
Hair is widely used in actual production.Due to the use of Cyanide Process, cyanide wastewater generally requires cycle Reusability,
This results in a large amount of depositions of the plurality of heavy metal such as copper, zinc, lead, manganese, cadmium, chromium in cyaniding tail washings, while there are organic in tail washings
Object and organic floating agent, feature may be summarized to be that high hypertoxic cyanide, high heavy metal, high organic matter, there are a small amount of carbon
Sulphur and silicate, and sometimes with a small amount of suspended matter and silt.This part cyaniding tail washings not only contains a certain amount of hypertoxic cyaniding
Object, it is often more important that the heavy metal ion containing a large amount of copper, zinc, lead, manganese, cadmium, chromium etc, if cannot effectively handle,
Pollution will be generated to natural environments such as water body, soil.Compare reason currently, also still lacking in terms of the processing of gold industry cyaniding tail washings
The copper thought, zinc, lead, manganese, cadmium, chromium mark feed method, solve the problems, such as this, will be produced to the science of gold industry, outside gold mining enterprises
The sustainable development of the real time monitoring of sewerage, the recycling of valuable noble metal, environment plays an important role.
There is provided copper in a kind of rapid and accurate determination cyaniding tail washings, zinc, lead, manganese, cadmium, chromium method will directly influence enterprise
The setting of technic index, and whether the discharge standard of meet the requirement of environmental protection, and either national standard, environmentally friendly ministerial standard at present
Or each place standard, all not no assay method about copper, zinc, lead, manganese, cadmium, chromium in gold industry cyaniding tail washings.It is only
National standard is also only the detection of conventional element in water quality, i.e. HJ766-2015《The measurement inductive coupling etc. of element in water quality 32
Ion emission spectroscopy method》、《The measurement Inductively coupled plasma-mass spectrometry of element in water quality 65》、HJ700-2014《In water quality 65
The measurement inductive coupling plasma emission spectrum method of element》、 GB7475-1987《Copper in Water, zinc, lead, Cadmium detrmination atom are inhaled
Receive spectrophotometry》, the range used is also only surface water, underground water, sanitary sewage and commonly industrial wastewater, in face of high acute
Malicious cyanide, high heavy metal, high organic matter cyaniding tail washings not have applicability.The high cyanide of cyaniding tail washings disappears in acid adding
Xie Shi will have hydrocyanic acid absorption plant, and be carried out under the sufficiently large draught cupboard of ventilation quantity, and wear safety device, to prevent hydrogen
Cyanic acid poisoning is dead, and the above method (HJ766-2015, HJ700-2014) does not do specific requirement, while acid adding amount in method
Less, the problems such as acid used is excessively single, digestion time is inadequate, sample treatment is not thorough enough can not also cope with Gao Chong in cyaniding tail washings
The objective fact of metal, high organic matter causes the resolution of cyaniding tail washings thorough.
Invention content
The present invention provides a kind of assay method of copper-lead zinc-manganese cadmium chromium in cyaniding tail washings, to solve high hypertoxic cyanide, height
Heavy metal, high organic matter, there are metal ions in the cyaniding tail washings of a small amount of carbon sulphur and silicate quick, Accurate Determining to show
Shape.
The technical solution adopted by the present invention is that including the following steps：
(1), 25mL cyaniding tail washings V are taken with graduated cylinder correct amount, are placed in 300mL conical flasks, 0.5-1g potassium chlorate is added,
0.2-0.5g ammonium acid fluorides connect hydrogen cyanide absorption plant, and nitric acid 5-8mL is added in acid-adding port, covers acid-adding port immediately later
Lid, shakes up to be placed on electric hot plate and heats 5-10min, and the hydrogen cyanide of generation is fully absorbed by the sodium hydroxide absorbing liquid of right end,
10-15mL nitric acid is added by acid-adding port again, lid lid is placed on electric hot plate heating and is removed slightly when clearing up to 8~10mL of volume
It is cold, remove hydrogen cyanide absorption plant；
(2), 5-8mL perchloric acid is added into the above-mentioned conical flask containing sample and 3-5mL sulfuric acid, cap upper surface ware adds
Heat resolution is removed slightly cold to close dry, 10mL nitric acid is added, washing table ware and bottle wall are placed on electric hot plate and heat 3-5min, make
Soluble-salt fully dissolves, and removes slightly cold；
(3), sample obtained by step (2) is transferred to 100mL volumetric flasks VxIn, deionized water is added and is settled to groove, shakes
It is even spare, it accurately pipettes 5mL samples with the mono- mark pipettes of 5mL and is placed in 100mL colorimetric cylinders, is i.e. extension rate f is 20, is added
10mL nitric acid is settled to groove with deionized water, shakes up to be measured；
(4), full procedure blank is done in company with sample, the wherein volume of sample to be tested blank is V0；
(5), the preparation of standard solution pipettes mixed standard solution 0mL, 5mL, 10mL, 15mL, 20mL and is placed in 100mL appearances
In measuring bottle, with 5% nitric acid constant volume, shake up spare；
(6), the measurement of sample, on inductively coupled plasma atomic emission spectrum, the spectral line for measuring tested element is strong
Degree deducts blank value, and tested element ρ is determined from working curvexAnd blank sample to be tested ρ0Mass concentration.
In the step (1), the nitric acid of addition is concentrated nitric acid, a concentration of 1.42g/mL.
In the step (2), the sulfuric acid concentration of a concentration of 1.67g/mL of perchloric acid of addition, addition are 1.67g/mL.
In the step (3), 100mL volumetric flasks are by calibrating qualified volumetric flask, and the mono- graticule pipettes of 5mL are to pass through
The pipette of calibration.
In the step (3), the nitric acid of addition is concentrated nitric acid, a concentration of 1.42g/mL.
In the step (5), mixed standard solution is national certified reference material, a concentration of 100ug/mL.
In the step (5), used 5% nitric acid, 5% refers to that volume ratio, nitric acid are the dense nitre of concentration 1.42g/mL
Acid.
In the step (6), metal element content calculation formula (1) to be measured is as follows in sample, calculates the amount for being tested element,
That is mass fraction ρ, numerical value are indicated with μ g/ml：
In formula：ρ-sample mass concentration, unit μ g/ml；
ρxThe mass concentration of-GOLD FROM PLATING SOLUTION category element to be measured, unit μ g/ml；
Vx- overall solution volume to be measured, units/ml；
ρ0The mass concentration of metallic element in-blank, unit μ g/ml；
V0- blank test solution total volume, units/ml；
F-extension rate；
V-sample point takes volume, units/ml.
This method first suitably stands cyaniding tail washings, then divides and 25mL cyaniding tail washings is taken to be placed in conical flask, this
Sample can to avoid in cyaniding tail washings with silt on the halfway influence of Specimen eliminating, 0.5-1g potassium chlorate, 0.2- is added
0.5g ammonium acid fluorides, sample connect hydrocyanic acid absorption plant, are placed in the sufficiently large draught cupboard of ventilation quantity, by acid-adding port plus
Enter appropriate nitric acid to be acidified, the hydrocyanic acid of generation imports sodium hydroxide solution absorption cell, neutralization reaction production by attachment device
Raw hydrocyanic acid, to avoid personal injury.Sample after acidification adds appropriate nitric acid, is thoroughly cleared up under the action of nitric acid
Sample, wherein nitric acid play leading oxidation, and when sample digestion is to about 10mL or so, appropriate perchloric acid and sulfuric acid, high chlorine is added
Acid and sulfuric acid play strong oxidation, can be to metal if there are organic matters in sample to eliminate organic matter and opening inclusion enclave
Ion generates suction-operated, if fruit, there are inclusion enclave, metal ion may be wrapped wherein, both situations can all cause
Measurement result is relatively low, is not thorough if sample still remains resolution after perchloric acid and sulfuric acid treatment is added, i.e., organic matter or
Black insoluble matter, then appropriate perchloric acid and sulfuric acid treatment sample will be continuously added, until Specimen eliminating is thorough, then steam to
It dips dry, slightly cold rear addition salt Ore Leaching, excessive hydrochloric acid forms complex with metal ion, and complex is very steady in the solution
It is fixed, be conducive to sample and measured on inductive coupling plasma emission spectrum.Its standard solution is the hybrid standard of each metal ion
Solution, by point taking and dilution is formulated step by step, system is uniform and stablizes.With inductive coupling plasma emission spectrum pair
When standard solution, blank and sample carry out analysis measurement, instrument is optimized, select suitable analysis spectral line, determined each
Instrument parameter, and then fast and accurately measure each tenor in cyaniding tail washings.This method successfully solves no national standard, row
The present situation measured specifically for Analysis of Heavy Metal Ions in gold industry cyaniding tail washings is marked, and according to cyaniding tail washings high toxicity, height
The characteristics of metal ion, high organic matter, there are a small amount of carbon sulphur and silicates, invention is effective, quickly and accurately analysis method,
It is easy to operate simultaneously, it can be achieved that sample batch operation, the real-time monitoring to the heavy metal ion content in cyaniding tail washings is valuable
The recycling of metal, the sustainable development important in inhibiting of environment.
Beneficial effects of the present invention：
1. for the own characteristic of gold industry cyanidation technology, invented it is a kind of it is accurate, quickly measure weight in cyaniding tail washings
The method of metal ion copper, lead, zinc, manganese, cadmium, chromium, filled up without national standard, environmentally friendly ministerial standard, each place standard can according to
Present situation provides accurate, timely important indicator for the qualified discharge of recycling and the environmental protection of gold mining enterprises metal ion.
2. for the high hypertoxic cyanide of cyaniding tail washings, high heavy metal, high organic matter, there are the spies of a small amount of carbon sulphur and silicate
Point, by hydrocyanic acid absorption plant, the hydrocyanic acid thoroughly generated to reaction absorbs, and avoids and is brought because hydrocyanic acid is poisoned
Human injury, the mesh thoroughly cleared up to metal ion, organic matter or adsorbate and, has been reached by the comprehensive functions of several acid
's.
3. potassium chlorate reagent is added, difficult decomposed substance in sample is decomposed as strong oxidizer, nitre is formed with nitric acid
Acid-potassium chlorate system, and then the carbon in sample, sulphur and organic adsorbents are removed, make in order to avoid it generates absorption to element to be measured
With influencing the accurate of measurement result.Ammonium acid fluoride reagent is added, can thoroughly open silicate sturcture, to eliminate because of silicate
Lower result phenomenon caused by package.Meanwhile the utilization perchloric acid and sulfuric acid of science thoroughly clear up sample, solve
High heavy metal, high organic matter cyaniding tail washings can not clear up thorough problem, and combine inductive coupling plasma emission spectrum pair
Heavy metal ion accurately and rapidly measures in sample.
4. this method is accurate, quickly, at the same it is easy to operate, it can be achieved that sample batch operation, effectively raise work
Efficiency.
Description of the drawings
Fig. 1 is hydrogen cyanide absorption plant figure.
Specific implementation mode
Embodiment 1
The unknown cyaniding tail washings of certain gold mining enterprises is selected as experimental subjects, it is carried out metal ion copper, lead, zinc, manganese,
The measurement of cadmium, chromium.
(1) 25mL cyaniding tail washings V are taken with graduated cylinder correct amount, be placed in 300mL conical flasks, 0.5g potassium chlorate, 0.2g is added
Ammonium acid fluoride connects hydrogen cyanide absorption plant, and nitric acid 5mL is added in acid-adding port, covers acid adding lid immediately later, shakes up postposition
In heating 5min on electric hot plate, the hydrogen cyanide of generation is fully absorbed by the sodium hydroxide absorbing liquid of right end, then is added by acid-adding port
Enter 10mL nitric acid, lid lid is placed on electric hot plate heating, when resolution remains 8mL to volume, removes slightly cold, removes hydrogen cyanide and absorb dress
It sets；
Aforesaid operations carry out under draught cupboard, and wear personal protection device, in case hydrogen cyanide causes personal injury, device
As shown in Figure 1, acid-adding port 1, reaction solution 2, sodium hydroxide solution 3 (a concentration of 5%, level 6-10cm), beaker 4
(500mL), conical flask 5 (300mL)；
(2) 5mL perchloric acid and 3mL sulfuric acid, cap upper surface ware, heating resolution are added into the above-mentioned conical flask containing sample
It to close dry, can not dry up, remove slightly cold, 10mL nitric acid be added, washing table ware and bottle wall are placed on electric hot plate and heat 3min, make
Soluble-salt fully dissolves, and removes slightly cold；
(3) upper step sample is transferred to 100mL volumetric flasks VxIn, deionized water is added and is settled to groove, shakes up spare, use
The mono- mark pipettes of 5mL accurately pipette 5mL samples and are placed in 100mL colorimetric cylinders, i.e. extension rate f is 20, and 10mL nitric acid is added, and is used
Deionized water is settled to groove, shakes up to be measured；
(4) full procedure blank is done in company with sample, the wherein volume of sample to be tested blank is V0；
(5) preparation of standard solution pipettes mixed standard solution 0mL, 5mL, 10mL, 15mL, 20mL and is placed in 100mL appearances
In measuring bottle, with 5% nitric acid constant volume, shake up spare；
(6) measurement of sample, on inductively coupled plasma atomic emission spectrum, the spectral line for measuring tested element is strong
Degree deducts blank value, and tested element ρ is determined from working curvexAnd blank sample to be tested ρ0Mass concentration；
By calculating, copper 1212.3mg/L, lead 909.6mg/L, zinc 812.7mg/L, manganese 1512.2mg/L, cadmium are measured
107.1mg/L, chromium 87.5mg/L.
Embodiment 2
The other unknown cyaniding tail washings of a gold mining enterprises is selected as experimental subjects, it is carried out metal ion copper, lead,
The measurement of zinc, manganese, cadmium, chromium.
(1) 25mL cyaniding tail washings V are taken with graduated cylinder correct amount, be placed in 300mL conical flasks, 0.8g potassium chlorate, 0.3g is added
Ammonium acid fluoride connects hydrogen cyanide absorption plant, and nitric acid 7mL is added in acid-adding port, covers acid adding lid immediately later, shakes up postposition
In heating 7min on electric hot plate, the hydrogen cyanide of generation is fully absorbed by the sodium hydroxide absorbing liquid of right end, then is added by acid-adding port
Enter 13mL nitric acid, lid lid is placed on electric hot plate heating, when about surplus 10mL of resolution to volume or so, removes slightly cold, removes hydrogen cyanide
Absorption plant；
Aforesaid operations carry out under draught cupboard, and wear personal protection device, in case hydrogen cyanide causes personal injury, device
As shown in Figure 1, acid-adding port 1, reaction solution 2, sodium hydroxide solution 3 (a concentration of 5%, level 6-10cm), beaker 4
(500mL), conical flask 5 (300mL)；
(2) 7mL perchloric acid and 4mL sulfuric acid, cap upper surface ware, heating resolution are added into the above-mentioned conical flask containing sample
It to close dry, can not dry up, remove slightly cold, 10mL nitric acid be added, washing table ware and bottle wall are placed on electric hot plate and heat 4min, make
Soluble-salt fully dissolves, and removes slightly cold；
(3) upper step sample is transferred to 100mL volumetric flasks VxIn, deionized water is added and is settled to groove, shakes up spare, use
The mono- mark pipettes of 5mL accurately pipette 5mL samples and are placed in 100mL colorimetric cylinders, i.e. extension rate f is 20, and 10mL nitric acid is added, and is used
Deionized water is settled to groove, shakes up to be measured；
(4) full procedure blank is done in company with sample, the wherein volume of sample to be tested blank is V0；
(5) preparation of standard solution pipettes mixed standard solution 0mL, 5mL, 10mL, 15mL, 20mL and is placed in 100mL capacity
In bottle, with 5% nitric acid constant volume, shake up spare；
(6) measurement of sample, on inductively coupled plasma atomic emission spectrum, the spectral line for measuring tested element is strong
Degree deducts blank value, and tested element ρ is determined from working curvexAnd blank sample to be tested ρ0Mass concentration.
By calculating, copper 512.2mg/L, lead 284.5mg/L, zinc 245.6mg/L, manganese 1345.8mg/L, cadmium are measured
85.2mg/L, chromium 86.2mg/L.
Embodiment 3
Include the following steps：
(1), 25mL cyaniding tail washings V are taken with graduated cylinder correct amount, be placed in 300mL conical flasks, 1g potassium chlorate, 0.5g fluorine is added
Change hydrogen ammonium, connect hydrogen cyanide absorption plant, nitric acid 8mL is added in acid-adding port, covers acid adding lid immediately later, shakes up and be placed on
10min is heated on electric hot plate, the hydrogen cyanide of generation is fully absorbed by the sodium hydroxide absorbing liquid of right end, then is added by acid-adding port
15mL nitric acid, lid lid are placed on electric hot plate heating and remove slightly cold when clearing up to volume 10mL, remove hydrogen cyanide absorption plant；
Aforesaid operations carry out under draught cupboard, and wear personal protection device, in case hydrogen cyanide causes personal injury, device
As shown in Figure 1, acid-adding port 1, reaction solution 2, sodium hydroxide solution 3 (a concentration of 5%, level 6-10cm), beaker 4
(500mL), conical flask 5 (300mL)；
(2), 8mL perchloric acid is added into the above-mentioned conical flask containing sample and 5mL sulfuric acid, cap upper surface ware, heating disappears
Solution can not dry up to close dry, remove slightly cold, and 10mL nitric acid is added, and washing table ware and bottle wall are placed on electric hot plate and heat 5min,
So that soluble-salt is fully dissolved, removes slightly cold；
(3), sample obtained by step (2) is transferred to 100mL volumetric flasks VxIn, deionized water is added and is settled to groove, shakes
It is even spare, it accurately pipettes 5mL samples with the mono- mark pipettes of 5mL and is placed in 100mL colorimetric cylinders, is i.e. extension rate f is 20, is added
10mL nitric acid is settled to groove with deionized water, shakes up to be measured；
(4), full procedure blank is done in company with sample, the wherein volume of sample to be tested blank is V0；
(5), the preparation of standard solution pipettes mixed standard solution 0mL, 5mL, 10mL, 15mL, 20mL and is placed in 100mL appearances
In measuring bottle, with 5% nitric acid constant volume, shake up spare；
(6), the measurement of sample, on inductively coupled plasma atomic emission spectrum, the spectral line for measuring tested element is strong
Degree deducts blank value, and tested element ρ is determined from working curvexAnd blank sample to be tested ρ0Mass concentration.
In 1~embodiment of embodiment 3：
In the step (1), the nitric acid of addition is concentrated nitric acid, a concentration of 1.42g/mL.
In the step (2), the sulfuric acid concentration of a concentration of 1.67g/mL of perchloric acid of addition, addition are 1.67g/mL.
In the step (3), 100mL volumetric flasks are by calibrating qualified volumetric flask, and the mono- graticule pipettes of 5mL are to pass through
The pipette of calibration.
In the step (3), the nitric acid of addition is concentrated nitric acid, a concentration of 1.42g/mL.
In the step (5), mixed standard solution is national certified reference material, a concentration of 100ug/mL.
In the step (5), used 5% nitric acid, 5% refers to that volume ratio, nitric acid are the dense nitre of concentration 1.42g/mL
Acid.
In the step (6), metal element content calculation formula (1) to be measured is as follows in sample, calculates the amount for being tested element,
That is mass fraction ρ, numerical value are indicated with μ g/ml：
In formula：ρ-sample mass concentration, unit μ g/ml；
ρxThe mass concentration of-GOLD FROM PLATING SOLUTION category element to be measured, unit μ g/ml；
Vx- overall solution volume to be measured, units/ml；
ρ0The mass concentration of metallic element in-blank, unit μ g/ml；
V0- blank test solution total volume, units/ml；
F-extension rate；
V-sample point takes volume, units/ml.
The effect further illustrated the present invention below by experimental example.
Experimental example 1
The accuracy of this method is verified due to unsuitable cyaniding tail washings standard specimen, so this experiment is using known to configuration
Concentration of analog sample simulates cyaniding tail washings, and then passes through the accuracy of experimental verification this method.
A kind of cyaniding tail washings 1000mL is simulated, wherein containing 10.0g gelatin, 3.0g Cymags, concentration of metal ions is copper
1000mg/L, lead 1000mg/L, zinc 1000mg/L, manganese 1000mg/L, cadmium 100mg/L, chromium 100mg/L.
(1) the above-mentioned simulation cyaniding tail washings V of 25mL are taken with graduated cylinder correct amount, be placed in 300mL conical flasks, 0.7g chlorine is added
Sour potassium, 0.4g ammonium acid fluorides connect hydrogen cyanide absorption plant, and nitric acid 6mL is added in acid-adding port, covers acid-adding port immediately later
Lid, shakes up to be placed on electric hot plate and heats 8min, the hydrogen cyanide of generation is fully absorbed by the sodium hydroxide absorbing liquid of right end, then is led to
It crosses acid-adding port and 12mL nitric acid is added, lid lid is placed on electric hot plate heating and removes slightly cold when clearing up to volume 10mL, removes cyaniding
Hydrogen absorption plant；
(2) 7mL perchloric acid and 4mL sulfuric acid, cap upper surface ware, heating resolution are added into the above-mentioned conical flask containing sample
It to close dry, can not dry up, remove slightly cold, 10mL nitric acid be added, washing table ware and bottle wall are placed on electric hot plate and heat 4min, make
Soluble-salt fully dissolves, and removes slightly cold；
(3) upper step sample is transferred to 100mL volumetric flasks VxIn, deionized water is added and is settled to groove, shakes up spare, use
The mono- mark pipettes of 5mL accurately pipette 5mL samples and are placed in 100mL colorimetric cylinders, i.e. extension rate f is 20, and 10mL nitric acid is added, and is used
Deionized water is settled to groove, shakes up to be measured；
(4) full procedure blank is done in company with sample, the wherein volume of sample to be tested blank is V0；
(5) preparation of standard solution pipettes mixed standard solution 0mL, 5mL, 10mL, 15mL, 20mL and is placed in 100mL appearances
In measuring bottle, with 5% nitric acid constant volume, shake up spare；
(6) measurement of sample, on inductively coupled plasma atomic emission spectrum, the spectral line for measuring tested element is strong
Degree deducts blank value, and tested element ρ is determined from working curvexAnd blank sample to be tested ρ0Mass concentration；
By calculating, copper 998.5mg/L, lead 995.4mg/L, zinc 1012.1mg/L, manganese 1010.6mg/L, cadmium are measured
95.5mg/L, chromium 94.8mg/L.With initial content copper 1000mg/L, lead 1000mg/L, zinc 1000mg/L, manganese 1000mg/L, cadmium
100mg/L, chromium 100mg/L are compared, and result is satisfactory result, and method is accurate and reliable.
Experimental example 2
Recovery testu is carried out to the unknown cyaniding tail washings in embodiment 1.
(1) the unknown cyaniding tail washings V in 25mL embodiments 1 is taken with graduated cylinder correct amount, be placed in 300mL conical flasks, is added
0.7g potassium chlorate is added in 25mg copper, lead, zinc, manganese and 2.5mg cadmiums, chromium, and 0.4g ammonium acid fluorides connect hydrogen cyanide absorption plant, in
Nitric acid 7mL is added in acid-adding port, covers acid adding lid immediately later, shakes up to be placed on electric hot plate and heat 8min, the cyaniding of generation
Hydrogen is fully absorbed by the sodium hydroxide absorbing liquid of right end, then 12mL nitric acid is added by acid-adding port, and lid lid is placed on electric hot plate and adds
Heat, resolution is to volume when remaining 10mL, removes slightly cold, removes hydrogen cyanide absorption plant；
(2) 7mL perchloric acid and 4mL sulfuric acid, cap upper surface ware, heating resolution are added into the above-mentioned conical flask containing sample
It to close dry, can not dry up, remove slightly cold, 10mL nitric acid is added, washing table ware and bottle wall are placed on electric hot plate and heat 3-5min,
So that soluble-salt is fully dissolved, removes slightly cold；
(3) upper step sample is transferred to 100mL volumetric flasks VxIn, deionized water is added and is settled to groove, shakes up spare, use
The mono- mark pipettes of 5mL accurately pipette 5mL samples and are placed in 200mL colorimetric cylinders, i.e. extension rate f is 40, and 20mL nitric acid is added, and is used
Deionized water is settled to groove, shakes up to be measured；
(4) full procedure blank is done in company with sample, the wherein volume of sample to be tested blank is V0；
(5) preparation of standard solution pipettes mixed standard solution 0mL, 5mL, 10mL, 15mL, 20mL and is placed in 100mL capacity
In bottle, with 5% nitric acid constant volume, shake up spare；
(6) measurement of sample, on inductively coupled plasma atomic emission spectrum, the spectral line for measuring tested element is strong
Degree deducts blank value, and tested element ρ is determined from working curvexAnd blank sample to be tested ρ0Mass concentration；
By calculating, copper 2209.5mg/L, lead 1897.8mg/L, zinc 1823.5mg/L, manganese 2545.6mg/L, cadmium are measured
204.5mg/L, chromium 184.5mg/L.Its rate of recovery be respectively copper 99.72%, lead 98.82%, zinc 101.1%, manganese 103.3%,
Cadmium 97.4%, chromium 97.0%, for the rate of recovery between 90%-110%, measurement result is satisfactory result, and above example proves this side
Method is feasible.
Claims (8)
1. the assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings, which is characterized in that include the following steps：
(1), 25mL cyaniding tail washings V are taken with graduated cylinder correct amount, be placed in 300mL conical flasks, 0.5-1g potassium chlorate, 0.2- is added
0.5g ammonium acid fluorides connect hydrogen cyanide absorption plant, and nitric acid 5-8mL is added in acid-adding port, covers acid adding lid immediately later, shakes
Even be placed on electric hot plate heats 5-10min, and the hydrogen cyanide of generation is fully absorbed by the sodium hydroxide absorbing liquid of right end, then is passed through
10-15mL nitric acid is added in acid-adding port, and lid lid is placed on electric hot plate heating and removes slightly cold when clearing up to 8~10mL of volume, removes
Hydrogen cyanide absorption plant；
(2), 5-8mL perchloric acid is added into the above-mentioned conical flask containing sample and 3-5mL sulfuric acid, cap upper surface ware, heating disappears
Solution is removed slightly cold to close dry, 10mL nitric acid is added, washing table ware and bottle wall are placed on electric hot plate and heat 3-5min, make solvable
Property salt fully dissolves, and removes slightly cold；
(3), sample obtained by step (2) is transferred to 100mL volumetric flasks VxIn, deionized water is added and is settled to groove, shakes up standby
With, accurately pipette 5mL samples with the mono- mark pipettes of 5mL and be placed in 100mL colorimetric cylinders, i.e. extension rate f be 20, be added 10mL nitre
Acid is settled to groove with deionized water, shakes up to be measured；
(4), full procedure blank is done in company with sample, the wherein volume of sample to be tested blank is V0；
(5), the preparation of standard solution pipettes mixed standard solution 0mL, 5mL, 10mL, 15mL, 20mL and is placed in 100mL volumetric flasks
In, with 5% nitric acid constant volume, shake up spare；
(6), the measurement of sample measures the intensity of spectral line for being tested element, button on inductively coupled plasma atomic emission spectrum
Except blank value, tested element ρ is determined from working curvexAnd blank sample to be tested ρ0Mass concentration.
2. the assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings according to claim 1, it is characterised in that：It is described
In step (1), the nitric acid of addition is concentrated nitric acid, a concentration of 1.42g/mL.
3. the assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings according to claim 1, it is characterised in that：It is described
In step (2), the sulfuric acid concentration of a concentration of 1.67g/mL of perchloric acid of addition, addition are 1.67g/mL.
4. the assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings according to claim 1, it is characterised in that：It is described
In step (3), 100mL volumetric flasks are by calibrating qualified volumetric flask, and the mono- graticule pipettes of 5mL are the liquid relief by calibration
Pipe.
5. the assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings according to claim 1, it is characterised in that：It is described
In step (3), the nitric acid of addition is concentrated nitric acid, a concentration of 1.42g/mL.
6. the assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings according to claim 1, it is characterised in that：It is described
In step (5), mixed standard solution is national certified reference material, a concentration of 100ug/mL.
7. the assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings according to claim 1, it is characterised in that：It is described
In step (5), used 5% nitric acid, 5% refers to that volume ratio, nitric acid are the concentrated nitric acid of concentration 1.42g/mL.
8. the assay method of copper-lead zinc-manganese cadmium chromium in a kind of cyaniding tail washings according to claim 1, it is characterised in that：It is described
In step (6), metal element content calculation formula (1) to be measured is as follows in sample, the amount of the tested element of calculating, i.e. mass fraction ρ,
Numerical value is indicated with μ g/ml：
In formula：ρ-sample mass concentration, unit μ g/ml；
ρxThe mass concentration of-GOLD FROM PLATING SOLUTION category element to be measured, unit μ g/ml；
Vx- overall solution volume to be measured, units/ml；
ρ0The mass concentration of metallic element in-blank, unit μ g/ml；
V0- blank test solution total volume, units/ml；
F-extension rate；
V-sample point takes volume, units/ml.
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| CN109839360A (en) * | 2019-01-23 | 2019-06-04 | 长春黄金研究院有限公司 | The measuring method of gold content in a kind of cyaniding tail washings |
| RU2718072C1 (en) * | 2019-08-23 | 2020-03-30 | Федеральное государственное автономное образовательное учреждение высшего образования «Северный (Арктический) федеральный университет имени М. В. Ломоносова» | Method of direct determination of lead in sea water |
| CN112782152A (en) * | 2019-11-06 | 2021-05-11 | 中国石油化工股份有限公司 | Method for detecting heavy metals in wastewater of refining and chemical device |
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