Method for determining rhenium in ores and ore concentrates by inverse volt-ampere measurements method

FIELD: chemistry.

SUBSTANCE: rhenium is transferred to solution, it is accumulated on golden-graphite electrode in mixed solution during 90-120 sec with electrolysis potentials (-0.7 ÷--1.0) V relatively to chlorine-silver electrode at background 1M HCl with following recording of anode pikes in executive volt-ampere diagrams filming mode with speed of potential reaming 30-50 mV/sec and concentration is determined on basis of pike height in spectrum of potentials from 0.700 to 0.800 V by method of attested mixtures addition.

EFFECT: higher efficiency.

2 ex, 2 tbl, 1 dwg

 

The invention relates to analytical chemistry, and in particular to methods for the determination of metal ions and can be used in hydrometallurgy, in different geological developments in the search and exploration in the case of the analysis of ores, as well as in the petrochemical industry for determining the content in solutions, ores and ore concentrates ions concentration of rhenium by Stripping voltammetry method (IIA).

Polarographic behavior of rhenium has been studied in solutions of acids (Hcl, lO4H2SO4N3RHO4, HNO3, acetic acid), in neutral solutions of the chlorides of potassium and sodium, and alkaline solutions [Lavoriamo, Animecon. Analytical chemistry of rhenium. - M.: Nauka, 1974. s].

The behavior of rhenium in sulphuric and phosphoric acid solutions. Geyer showed [Gr THIS anorg. allgem. Chem., 263, 47 (1950)], the number of waves of recovery and their character will change depending on the concentration of H2SO4. The half-wave potential for E1/2for rhenium (VII) 3.5 M H2SO4equal to from 0.2 to -0,45 C. In this case, the determination of rhenium interfere with the anions CL-NO

-
3
, PO
3-
4
and Mo, Fe and Ti.

The behavior of rhenium is neutral, alkali and buffer solutions. The use of polarographic in neutral and alkaline solutions most appropriate for the determination of small concentrations of rhenium [Rubinsky TA, Miranowski YEAR electrochemistry, 7, 1403 (1971)]. Catalytic wave, suitable for analytical purposes, the answer from -1,2 up -1,6 C. In this process, preventing the influence of ions CL-NO

-
3
SO
2-
4
, PO
3-
4
and Mo, cu, Zn, Cd, Pb, Bi, Se, Co, and W.

The behavior of rhenium in solutions of nitric acid. Oscillographic method made it possible to observe the cathodic wave recovery of rhenium. 1 M NGO3the half-wave potential for the rhenium is equal to minus 0.6 C. the detection limit was 10-3-10-4%. Interfering elements are Mo, cu, Zn and W, and the anions CL-and other

The behavior of rhenium in hydrochloric and homocyclic solutions. Maximum wave height recovery of rhenium occurs in 2-4,3 M Hcl [Lingune J.J. SOC., 64, 1001, 2182 (1942); 65, 866 (1943)]. The half-wave potential for E1/2for rhenium (VII) in 2 M Hcl equal -0,45 In, and 4.2 M Hcl 0.31 Supranational Century Under taccom this process is what is the definition of rhenium prevent ions NO

-
3
SO
2-
4
, PO
3-
4
that distort the line of the background, as well as molybdenum and tungsten, which are associated elements rhenium ores and ore concentrates.

Known polarographic methods for the determination of rhenium, which are divided into 2 groups:

a) methods for the determination of large quantities (10-3% and above), based on the measurement of waves restore perrenate;

b) methods for the determination of micro-amounts of rhenium in the range of 10-3-10-7using catalytic currents and the concentration of rhenium on the electrode in the form of poorly soluble film of oxide.

The content of rhenium in the alloy from 2· 10-1% and more usually dened by the wave with E1/2=-0,3-0,4 Century against the background of 2.5 M H2SO4. Smaller amounts of rhenium (up to 10-3%) in products of copper and molybdenum production is determined by the catalytic wave of hydrogen with E1/2=-1,2 on the background of phosphate buffer solution (pH 7-8). The disadvantage of this method is that the molybdenum p is evritania separated in the form of insoluble calcium molybdate sintering samples with Cao at 600-700° C for 2 h Detailed course analysis given in [Kryukov T.A., siniakova SR, Aref'eva T.V. Polarographic analysis. M: Goskomizdat, 1959, s].

Molybdenum concentrates, it is recommended to also decompose conc. HNO3with subsequent distillation Re2O7from sulfuric acid solution [Duca, A., Stanescu D., M. Puscasu the Parliament of the si cercetari chim. Acad. RPR Fil. Cluj, 6, 123 (1955); 13, 197 (1962)]. Determination of rhenium conducted against the backdrop of NaCl+Na2SO3(pH of 11.3-11,5) at a molar ratio of Mo:Re≤ 200:1 and E1/2=-0,45 Century Opened a minimum of 1-2 g Re/ml. Determination carried out after sample preparation, during which rhenium is separated molybdenum, tungsten and other related items.

Sensitive method is Stripping voltammetric method for the determination of rhenium in the background 4M N2RHO4using oscillographic polarography and mercury stationary microelectrode [A. M. Demkin, siniakova SR SB. Determination of trace contaminants. M: DNTP, 1968, p.31] (prototype). Determination of rhenium carried out by the following method. Aliquot part 5-10 ml (4 M H3RHO4), containing ~ 0.01 to 0.1 g Re, placed in the electrolytic cell. Within 3 minutes through a solution of nitrogen purge, set on the oscilloscope polarography mode anodic polarization and potential mercury microelectrode set to 0.95 Century Record wave when idempotence. A necessary condition of the process is that the rhenium in the samples is separated from molybdenum and tungsten. This condition is one of the drawbacks of this method.

The main task of the proposed solution is the determination of rhenium in ores and ore concentrates on graphite electrode by the method of WILLOW.

This object is achieved in that the rhenium electrochemically concentrate on different types of graphite electrodes (impregnowana graphite (IG), mercury-graphite (WG), silver-graphite (SG) or gold-graphite (ZG)) with the subsequent registration of the anode voltamperes. The new method is that spend the accumulation of rhenium in the mixed solution within 90-120 s potential electrolysis Ee=(a-0.7 ÷ -1,0) In the background: 1 M Hcl, followed by registration anodic peaks in the accumulation mode shooting voltamperes at scan rate of 30-50 mV/C. the Concentration of rhenium is determined by the height of the anodic peak in the range of potentials from 0,700 to 0.800 to relatively busy chloridizing electrode (us. H. E.).

In the prototype, the quantitative determination of rhenium based on response and recovery is only possible after careful separation from molybdenum, which is often associated with the element rhenium in ores and ore concentrates.

In the proposed method the first time the s installed capacity of rhenium to oxidize at different types of graphite electrodes. As the indicator used IG, SG, WG and ZG electrodes (in the prototype used mercury-drop electrode). The use of such electrodes due to the high chemical and electrochemical stability of graphite, a wide range of working potentials, as well as the simplicity of a manual update of the surface and safety. In addition, the WG electrode significantly reduces the consumption of mercury.

The maximum value of the detected current is observed in ZG electrode. IG and IG electrodes are also suitable for use, however, due to the large residual currents they were less convenient than ZG electrode. The CR electrode reproducibility of the analytical signal is not satisfactory and this raises the need for mechanical cleaning of the electrode, which is also reflected on the analytical signal. ZG electrode was first used for the determination of rhenium in ores and ore concentrates.

In the prototype described using as background 4M solution of phosphoric acid. In these conditions it is possible to identify only large quantities of rhenium (~ 10-2%). When determining the amounts of rhenium in these conditions it is necessary to distinguish from complex structures, as most of the associated elements are interfering (for example, molybdenum, tungsten and copper). PR is alagaesia in the invention backgrounds 1 M H 2O2or 0.5 M HNO3or 0.5 M HCOOH, or 1 M Hcl allow us to determine the rhenium with good reproducibility. The use of background 0.5 M NGO3hampered by the fact that for the determination of rhenium was observed sufficiently large residual current, and when using backgrounds 1 M H2About2and 0.5 M HCOOH is impossible to determine the rhenium in the presence of molybdenum, as these backgrounds analytical signal molybdenum mutes analytical signal rhenium. The highest sensitivity was observed on the background of 1 M Hcl in ZG electrode. Using this background also solves the problem of joint determination of rhenium and molybdenum. The detection limit is 10-6-10-2% (in the prototype 10-3-10-2%).

The gold concentration significantly affects the peak current of rhenium. The drawing shows that when CAI=1· 10-4mg/l sensitivity factor is significantly higher than when CAu=1· 10-5mg/L. Thus, we proposed that the definition of rhenium on ZG electrode CAu=1· 10-4mg/L. Further increasing the concentration of gold is impractical because a large current gold mutes the current rhenium.

The results of the use of different electrodes on different backgrounds are shown in table 1. The table shows that ZG electrode the highest sensitivity coefficients. The same pattern is observed if the definition is on the background of 1 M Hcl, moreover, against this background, it is possible to quantify the rhenium in the presence of molybdenum. Thus, we have proposed definition of rhenium and rhenium in the presence of molybdenum in ZG electrode and on the background of 1 M Hcl.

The measurement results of the analytical signal of rhenium on ZG electrode are given in table 2. As can be seen from the table, the measurement error is about 5%. The calculation determined the concentration of rhenium is carried out according to the method introduced is found." The difference is that the current peak gold is subtracted from the analytical signal was measured at a potential of Ee=0,700÷ 0.800 to Century

The pre-electrolysis (τe) is selected depending on the concentration of the detected substance. The maximum value of the current magnitude of oxidation is achieved when the τeequal 90-120 sec. At τeless than 90 decreases the detection sensitivity and increases the error of the determination, and when τemore than 120 decreases expressnet.

Important for the determination of rhenium is the selection of the scan rate of the potential. The optimum speed 30-50 MB/s speed Increase of more than 50 mV/s increases the sensitivity, but this increases the residual current and the resolution decreases. Using speed 30 MB/s significantly reduces the magnitude of the anode current and reduced sensibility the determination of rhenium.

Thus, the established conditions for the first time allowed us to quantify the rhenium ores and ore concentrates on the basis of the reaction of electrooxidation. To increase the sensitivity of the definitions used pre-concentration of rhenium on the surface of graphite electrodes. The proposed voltammetric method will significantly improve the detection sensitivity (1· 10-6mg/kg), which is 3-4 orders of magnitude lower compared to the prototype, the analysis time does not exceed 90-120 s, versus 30 minutes for the Definition does not interfere with molybdenum, tungsten and copper, which are related elements in ores and ore concentrates.

As a prototype of the selected method for the determination of rhenium in current-voltage curves of the electroreduction Re(7+)→ Re(4+). Our proposed definition of rhenium method IIA, which is electroencephalogra rhenium gold graphite electrode with subsequent oxidation of the sediment. The analysis was performed on the device STA-1 (Tomsk, Russia). The chosen method allows to significantly extend the range of the defined concentrations from 10-3-10-2up to 10-6-10-2%, and also allows to simplify the instrumentation process. In addition, this method allows to determine the rhenium in the presence of molybdenum, which resolves the issues of preparation of the sample for which the analysis.

Examples of specific performance:

Example No. 1. Measurements were carried out on artificial mixtures. 10 ml of background electrolyte is placed in a quartz glass. Stopping stirring, carry out the electrolysis of a solution under the condition: Ee=-0,800, τe=90 C. Remove the current-voltage curve of the electrooxidation at scan rate of 40 mV/s, since the potential of Ebeg=0,001 Century, the Absence of peaks indicates the purity of the background. Then add 0.05 ml standard sample (CO) gold and spend electrochemical sediment concentration under similar conditions. The peak for the specified concentration of a substance recorded in the range of potentials from 0,700 to 0.800 to In (relative to the us. H. E.). Added 0.05 ml WITH rhenium and again recorded the analytical signal. Did 0,05 ml additive WITH rhenium and shot the volt-ampere curve of the electrochemical oxidation of the sediment. According to the difference of the currents peaks rhenium calculated the concentration of rhenium in the solution. A distinctive feature is that of the analytical signal was measured at a potential of Ee=0,700÷ 0.800 to read In the current peak gold (background line). Determination of rhenium in the presence of molybdenum is the same but the background electrolyte is added molybdenum (from 0.05 to 5 ml WITH molybdenum). It is established that at 1000-fold excess of molybdenum (compared with rhenium) rhenium you can define the number is significant. WITH rhenium was obtained by diluting 0.05 g of powder of pure rhenium in 50 ml of a solution containing 25 ml of concentrated NGO3and trichitillomania water. WITH molybdenum was obtained in the same way. WITH gold prepared from fixanal by diluting 1 M Hcl. The background electrolyte was obtained by dilution of concentrated hydrochloric acid (84 ml conc. HCl in a volumetric flask 100 ml). Measurement error is of the order of 1-5% (table. 2).

Example 2. 0.1 g. powder catalyst containing rhenium, was dissolved in 15% HNO3in the flask 100 ml for 15-20 minutes under stirring. 10 ml of background electrolyte were placed in a quartz glass was added to 0.1 ml WITH gold. Registered analytical signal electrooxidation of gold. Added aliquot part 1-1,5 ml of the resulting solution of catalyst. Filmed volt-ampere curve of the electrochemical oxidation of rhenium. Did Supplement WITH rhenium 1 ml and again recorded the analytical signal. According to the difference of the currents peaks rhenium calculated the concentration of rhenium in the solution. Peak current measurements were recorded at a potential of E=0,750 Century the Concentration of rhenium was ~ 65%. WITH rhenium, gold, and the background electrolyte is prepared as in example 1.

Thus, the first set of the ability of quantitative analysis of rhenium on the peaks of its oxidation on MO electrode (in the prototype quantitative determination of rhenium Provo is Yat wave recovery on a mercury drop electrode). Increased detection sensitivity (more than 2-3 orders of magnitude). The conditions used in the prototype, does not allow an analysis of the rhenium in the presence of molybdenum.

The proposed method is simple, significantly reduces the use of toxic mercury, does not require much labour, a large number of reagents and can be used in any chemical laboratory with computerized analyzers type STA, TA or polarograph. The proposed method can be used for the determination of rhenium in ores and ore concentrates.

Table 1
The sensitivity coefficients of the various electrodes on different background electrolytes
ElectrodeSensitivity coefficients for different background electrolytes
 H2O2HNO3HCOOHHCl
Impregnated graphite0,6060,4370,2000,771
Mercury-graphite0,5610,301 0,2540,211
Gold-graphite0,6120,4410,4120,804
Silver-graphite0,6090,3920,3010,692
Table 2
"Put-found" for the determination of rhenium in ZG electrode with the following parameters:Au=1· 10-4mg/l; τe=90; von 1 M Hcl; Fp=0,750
no experienceWithR·105g/l inputEeInWithRe·105mg/l, definedError, %
12,000,7521,981,00
24,000,7483,824,50
36,000,7495,911,50
48,000,7517,990,12
510,000,75010,021,96

The method of determination of rhenium in ores and ore concentrates by Stripping voltammetry method, which consists in the fact that rhenium is transferred from the sample in the solution and hold voltammetric determination, wherein spend the accumulation of rhenium on Zolotaryova electrode in a mixed solution within 90-120 s potential electrolysis (a-0.7) ÷-(-1,0) In a relatively saturated chloridizing electrode on the background of 1 M Hcl followed by registration anodic peaks in the accumulation mode shooting voltamperes at scan rate of the potential of 30-50 mV/s and the concentration is determined by the peak height in the range of potentials 0,700 - 0.800 to In method of additives certified mixtures.



 

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