Novel combined alkali flux and chemical analysis method using novel combined alkali flux

Abstract

The invention discloses a novel combined alkali flux and a chemical analysis method using the novel combined alkali flux, the novel combined alkali flux comprises sodium peroxide and sodium hydroxide, and the mass ratio of the sodium peroxide to the sodium hydroxide is 3.5: 0.5-2.8: 1.2. Placing a to-be-detected ore sample in an iron crucible or a corundum crucible, uniformly mixing the combined alkali flux according to the proportion, adding 3g of the combined alkali flux into the vessel, uniformly stirring, covering 1g of the combined alkali flux, covering, placing in a high-temperature furnace which is heated to 650 DEG C in advance, heating to 700 DEG C, and keeping for 5-7 minutes until a melt is in a full melting state. When the combined alkali flux is used, the use amount of sodium peroxide can be effectively reduced, and the chemical analysis cost is reduced.

Description

Technical Field

[0001] The present invention belongs to the technical field of chemical analysis, and particularly relates to a novel combined alkali flux and a chemical analysis method using the novel combined alkali flux. Background Art

[0002] In the related prior art, the analytical method for tungsten trioxide in process ore samples is "Determination of tungsten content by thiocyanate photometric method - GB / T 14352.1—2010". It involves using the oxidizing alkali flux sodium peroxide to melt the sample at high temperature. Sodium peroxide is an explosive precursor hazardous chemical and is expensive. Therefore, a research project on novel alkali flux technology is carried out. While maintaining the accuracy of analysis and detection, if the amount of sodium peroxide used can be reduced, the analysis and detection cost can be effectively reduced. Summary of the Invention

[0003] To solve the above technical problems, the present invention provides a novel combined alkali flux and a chemical analysis method using the novel combined alkali flux. The novel combined alkali flux can effectively reduce the amount of sodium peroxide used and lower the detection cost.

[0004] One object of the present invention is to provide a novel combined alkali flux, which includes sodium peroxide and sodium hydroxide, and the mass ratio of sodium peroxide to sodium hydroxide is 3.5:0.5 to 2.8:1.2.

[0005] As a preferred embodiment, the mass ratio of sodium peroxide to sodium hydroxide is 3:1 to 2.8:1.2.

[0006] As a preferred embodiment, the mass ratio of sodium peroxide to sodium hydroxide is 3:1.

[0007] Another object of the present invention is to provide a chemical analysis method using the novel combined alkali flux, which uses the combined alkali flux and determines the tungsten content according to the method in the national standard GB / T 14352.1—2010.

[0008] As a preferred embodiment, the ore sample to be tested is placed in an iron crucible or a corundum crucible. After the combined alkali flux is mixed evenly according to the above mass ratio, a first mass of the combined alkali flux is taken and added to the above vessel and stirred evenly, and then a second mass of the combined alkali flux is covered. After covering the lid, it is placed in a preheated high-temperature furnace for melting.

[0009] As a preferred embodiment, the sum of the first mass and the second mass is 4 g, and the mass ratio of the first mass to the second mass is 3:1 to 2.5:1.5.

[0010] As a preferred solution, place the ore sample to be measured in an iron crucible or a corundum crucible. After mixing the combined alkali flux evenly according to the mass ratio of 3:1 to 2.8:1.2, take 3 g of the combined alkali flux and add it to the above-mentioned vessel and stir evenly. Then cover it with 1 g of the combined alkali flux. After covering, place it in a high-temperature furnace preheated to 650 °C, heat it to 700 °C and keep it for 5 min to 7 min until the melt just becomes completely molten.

[0011] Compared with the prior art, the present invention has at least the following beneficial effects:

[0012] First, the present invention provides a novel combined alkali flux. Through a large number of experiments and analyses, a reagent that can effectively cooperate with sodium peroxide in the oxidation alkali flux and also achieve efficient separation of the sample is found. When using the combined alkali flux of this solution, the amount of sodium peroxide used can be effectively reduced, and the chemical analysis cost can be reduced. During the sample melting process for the determination of tungsten content by the thiocyanate photometric method in the national standard GB / T 14352.1—2010, the mass of the novel combined alkali flux used is the same as that of sodium peroxide in the oxidation alkali flux in the original method. The cost of this novel combined alkali flux is 23% lower than that of the single oxidation alkali flux sodium peroxide. Therefore, the chemical analysis cost can be effectively reduced.

[0013] Second, the present invention also provides a chemical analysis method for detecting tungsten trioxide in a combined alkali flux for melting ore samples. In the process of using the above-mentioned novel combined alkali flux to melt ore samples for the chemical analysis method of detecting tungsten trioxide, no new impurity ions are introduced, and the fluid smoothness during the melting of the novel combined alkali flux is relatively good. The stability of the analysis and detection results for tungsten trioxide is within the error range, and the coincidence degree is relatively high. Specific Embodiments

[0014] In order to make the technical means, creative features, achieved purposes and beneficial effects of the present invention easy to understand, the present invention will be further described below in conjunction with specific embodiments.

[0015] In addition, in order to better illustrate the present invention, numerous specific details are given in the following specific embodiments. Those skilled in the art should understand that the present invention can also be implemented without some specific details. In other embodiments, methods, means, equipment and steps well known to those skilled in the art are not described in detail in order to highlight the main idea of the present invention.

[0016] This embodiment provides a novel combined alkali flux, which includes sodium peroxide and sodium hydroxide, and the mass ratio of sodium peroxide to sodium hydroxide is 3.5:0.5 to 2.8:1.2. Preferably, the mass ratio of sodium peroxide to sodium hydroxide is 3:1 - 2.8:1.2. More preferably, the mass ratio of sodium peroxide to sodium hydroxide is 3:1. Considering the need for detection cost, in the single - detection dosage, the total mass of sodium peroxide and sodium hydroxide is 4 g.

[0017] This embodiment also provides a chemical analysis method for detecting tungsten trioxide in a combined alkali flux for melting ore samples, which includes the following steps: Place the ore sample to be tested in a vessel (iron crucible or corundum crucible). After mixing the combined alkali flux (sodium peroxide and sodium hydroxide) evenly according to the mass ratio of 3:1 (sodium peroxide:sodium hydroxide), take 3 g of the above - mixed combined alkali flux and add it to the above - mentioned vessel and stir evenly, then cover it with 1 g of the above - mentioned combined alkali flux. After covering the lid, place it in a high - temperature furnace pre - heated to 650 °C, heat it to 700 °C and keep it for 5 min - 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0018] The subsequent steps are all detected according to the detection steps of the thiocyanate photometric method in the national standard GB / T 14352.1—2010 to determine the tungsten content. It should be noted that the difference between this scheme and the national standard detection method is only: the combined alkali flux and its ratio, and other parts refer to the detection method of the national standard GB / T 14352.1—2010.

[0019] In the following examples and comparative examples of this scheme, through summarizing the reagent screening, reagent ratio, addition method and melting phenomenon of the novel combined alkali flux, the chemical analysis method of "mixing the novel combined alkali flux of sodium hydroxide + sodium peroxide evenly according to the mass ratio of 1:3 (sodium hydroxide:sodium peroxide), adding 3 g in the ore sample melting vessel, weighing the sample, shaking it evenly, and then covering it with 1 g and then carrying out melting" is determined, which has a stable analysis accuracy rate. The following examples and comparative examples use the chemical analysis method of melting ore samples with the novel combined alkali flux to detect tungsten trioxide. During the process, no new impurity ions are introduced, and the fluid smoothness during the melting of the novel combined alkali flux is relatively good. The stability of the analysis and detection results for tungsten trioxide is within the error range, and the degree of coincidence is relatively high.

[0020] Comparative Examples 1 - 8

[0021] When melting ore samples with sodium peroxide, the series of indexes during the melting of 8 groups of ore samples according to the national standard "Determination of Tungsten Content by Thiocyanate Photometric Method GB / T 14352.1—2010" are as follows: Among them, the recovery rate = [crude concentrate grade * (raw ore grade - tailing grade)] / [raw ore grade * (crude concentrate grade - tailing grade)]; the enrichment ratio = crude concentrate grade / raw ore grade. As shown in Table 1.

[0022] Table 1 Series of indicators when using sodium peroxide alone to melt ore samples

[0023]

[0024] Examples 1 - 8

[0025] The differences from Comparative Examples 1 - 8 are only as follows: A new type of combined alkali flux (sodium hydroxide: sodium peroxide mixed evenly at a mass ratio of 1:3) is used. 3 g of the combined alkali flux is added into the ore sample melting vessel. After weighing and shaking the sample evenly, another 1 g of the combined alkali flux is covered and then melting is carried out. As shown in Table 2.

[0026] Table 2 Series of indicators when using the combined alkali flux to melt ore samples

[0027]

[0028]

[0029] Table 3 Average differences in series of indicators between melting with the combined alkali flux and melting with sodium peroxide alone

[0030] Project Raw ore % Rough concentrate % Tailings % Recovery rate % Enrichment ratio Combined agent 0.0574 1.094 0.0145 75.74 19.06 Sodium peroxide 0.0572 1.101 0.0143 75.99 19.25 Difference 0.0002 -0.007 0.0002 -0.25 -0.19

[0031] From the above data in Tables 1 - 3, it can be seen that the differences in the average of the original ore, the average of the rough concentrate, the average of the tailings, the average of the recovery rate, and the average of the enrichment ratio of the series of ore samples melted with the combined alkali flux in Examples 1 - 8 compared with those melted with sodium peroxide as the single oxidation alkali flux in Comparative Examples 1 - 8 are not obvious. The stability of the analysis accuracy is within the error range, and the degree of coincidence is relatively high.

[0032] The following is the cost accounting of the chemical analysis and detection methods for Examples 1 - 8: Sodium peroxide belongs to an explosive precursor under controlled management. Each barrel is 500 g, and the market price is 130.00 yuan / barrel; sodium hydroxide is 500 g per bottle, and the market price is 12.00 yuan / bottle. After applying the chemical detection method of the present invention, the cost of the combined alkali flux is reduced by about 23% compared with that of sodium peroxide as the single oxidation alkali flux.

[0033] Comparative Examples 9 - 11

[0034] When using sodium peroxide to melt ore samples, the series of indicators for melting 8 groups of ore samples in accordance with the national standard GB / T 14352.1 - 2010 are as follows:

[0035] The differences from Comparative Examples 1 - 8 are only as follows: The ore samples detected are different.

[0036] Phenomena during the melting and sample analysis process: Sodium peroxide alone: It is easy to melt, the surface is smooth after melting, and there will be visible particulate matters when the sample amount is large (which does not affect the analysis result), and the melted minerals fall off quickly when taking 2% ethanol solution.

[0037] Comparative Examples 12 - 14

[0038] The difference from Comparative Examples 9 - 11 is as follows: Replace the single sodium peroxide flux with a combined flux of sodium peroxide / sodium carbonate, where sodium peroxide and sodium carbonate are mixed evenly at a mass ratio of 3:1. Take 3 g of the above combined flux (sodium peroxide and sodium carbonate) and add it to the above vessel and stir evenly. Then cover it with 1 g of the above combined flux, cover the lid, place it in a muffle furnace preheated to 650 °C, heat it to 700 °C and keep it for 5 min - 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0039] Subsequent steps are all detected in accordance with the national standard GB / T 14352.1—2010.

[0040] It should be noted that the difference in the national standard detection method between this Comparative Example 12 - 14 and Comparative Examples 9 - 11 is only that: the components of the above - mentioned combined flux (sodium peroxide and sodium carbonate) are different, and other parts refer to the national standard detection method.

[0041] Phenomena during the melting and sample analysis process of Comparative Examples 12 - 14: Using the combined flux of sodium peroxide / sodium carbonate: It is easy to melt, the surface is smooth after melting. When extracting with 2% ethanol solution, the molten minerals fall off slightly slower than when using only sodium peroxide, and they fall off completely after about 1 minute. During the process of volume - fixing and mixing of the color - developing solution, a large number of bubbles will overflow, impacting the bottle cap and causing the color - developing acid solution to splash.

[0042] Examples 9 - 11

[0043] The difference from Comparative Examples 9 - 11 is as follows: Replace the single sodium peroxide flux with a combined flux of sodium peroxide / sodium hydroxide, where sodium peroxide and sodium hydroxide are mixed evenly at a mass ratio of 3:1. Take 3 g of the above combined flux (sodium peroxide and sodium hydroxide) and add it to the above vessel (iron crucible or corundum crucible) and stir evenly. Then cover it with 1 g of the combined flux, cover the lid, place it in a muffle furnace preheated to 650 °C, heat it to 700 °C and keep it for 5 min - 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0044] Subsequent steps are all detected in accordance with the national standard GB / T 14352.1—2010.

[0045] The difference in the national standard detection method between this Example 9 - 11 and Comparative Examples 9 - 11 is only that: the above - mentioned combined flux (sodium peroxide and sodium hydroxide) is different, and other parts refer to the national standard detection method.

[0046] Phenomena during melting and sample analysis: When using the sodium peroxide / sodium hydroxide combined flux in this application, it is easy to melt, the surface is smooth after melting, and when taking 2% ethanol solution, the molten minerals fall off slightly slower than when using all sodium peroxide, and they fall off completely after about 1 minute of standing.

[0047] Table 4 Verification condition settings for the melting process of the combined flux in the screening of combined flux agents

[0048] Item Flux name Dosage Combined ratio Set temperature for high-temperature melting Comparative examples 9 - 11 Sodium peroxide 4g All 700℃ Comparative examples 12 - 14 Sodium peroxide / Sodium carbonate 4g 3 / 1 700℃ Examples 9 - 11 Sodium peroxide / Sodium hydroxide 4g 3 / 1 700℃

[0049] Table 5 Comparison of the results of decomposing ore samples by flux agents

[0050]

[0051]

[0052] According to the content of Tables 4 - 5 above and the phenomena during melting and sample analysis, it can be seen that when comparing Comparative Examples 9 - 11, Comparative Examples 12 - 14 and Examples 9 - 11, the analysis results of the same sample by the single sodium peroxide flux, sodium peroxide / sodium carbonate combined flux, and sodium peroxide / sodium hydroxide combined flux are all within the allowable error range, and the degree of coincidence is relatively high. However, during the analysis operation process, when using the combined flux (sodium peroxide and sodium carbonate) in Comparative Examples 12 - 14, a large amount of gas will overflow after decomposition, and there is a safety hazard when shaking the color-developing solution evenly. Therefore, the combined flux (sodium peroxide and sodium carbonate) has poor effects; in Examples 9 - 11, the sodium peroxide / sodium hydroxide combined flux is used, which is similar in properties to the total use of sodium peroxide flux in Comparative Examples 9 - 11 during the ore sample melting and analysis process. Therefore, the sodium peroxide / sodium hydroxide combined flux in Examples 9 - 11 is feasible as a substitute flux.

[0053] Blank verification of combined alkali fusion high-temperature decomposition reagent

[0054] Definition of reagent blank: Use blank (without adding ore sample) to replace the reagent sample, and perform the determination according to the same analysis steps as the reagent sample to eliminate possible background interferences such as experimental water, reagents, environmental humidity, etc. during the detection process, and ensure the accuracy and reliability of the experimental results. As shown in Tables 6 and 7.

[0055] Comparative Examples 15 - 19

[0056] The difference from Comparative Examples 1 - 8 is only that: no sample is added to the vessel.

[0057] Examples 12 - 16

[0058] The difference from Comparative Examples 15 - 19 is only that: the combined flux: sodium peroxide / sodium hydroxide is used.

[0059] That is, the combined flux (sodium peroxide and sodium hydroxide) is mixed evenly according to the mass ratio of 3:1 (sodium peroxide: sodium hydroxide). After that, 3 g of the evenly mixed combined flux is taken and added into a vessel (iron crucible or corundum crucible), and stirred evenly. Then, 1 g of the above combined flux is covered. After covering the lid, it is placed in a high-temperature furnace preheated to 650 °C, heated to 700 °C and maintained for 5 min to 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0060] The measurement method steps are all detected in accordance with the national standard GB / T 14352.1—2010.

[0061] Table 6 Condition settings for the verification process of the alkaline combined flux reagent blank

[0062] Item Flux name Dosage Combined ratio Set temperature for high-temperature melting Comparative examples 15 - 19 Sodium peroxide 4g All 700℃ Examples 12 - 16 Sodium peroxide / Sodium hydroxide 4g 3 / 1 700℃

[0063] Table 7 Comparison results of the combined flux and the reagent blank results of all sodium peroxide melts

[0064]

[0065]

[0066] The results show that under the same experimental conditions, the combined fluxes of Examples 12-16 and the reagent blank values of the comparative examples 15-19 using all sodium peroxide melts are consistent. Therefore, the following conclusion can be obtained: When the combined flux (sodium peroxide / sodium hydroxide) is melted at high temperature, it will not affect the analysis results due to the change of its own reagent.

[0067] Comparative examples 20-28

[0068] The difference from Comparative examples 1-8 is only that: the ore samples to be detected are different.

[0069] Examples 17-25

[0070] The difference from Comparative examples 20-28 is only that: the combined flux uses sodium peroxide / sodium hydroxide.

[0071] That is, the ore sample to be detected is placed in a vessel (iron crucible or corundum crucible). The combined flux (sodium peroxide and sodium hydroxide) is mixed evenly according to the mass ratio of 3:1 (sodium peroxide: sodium hydroxide). After that, 3 g of the evenly mixed combined flux is taken and added into the above vessel and stirred evenly. Then, 1 g of the above combined flux is covered. After covering the lid, it is placed in a high-temperature furnace preheated to 650 °C, heated to 700 °C and maintained for 5 min to 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0072] The measurement method steps are all detected in accordance with the national standard GB / T 14352.1—2010.

[0073] Examples 26 - 34

[0074] The difference from Comparative Examples 20 - 28 is only that: the alkali flux uses a sodium peroxide / sodium hydroxide combined alkali flux.

[0075] That is, place the ore sample to be measured in a vessel (iron crucible or corundum crucible). After mixing the combined alkali flux (sodium peroxide and sodium hydroxide) evenly according to the mass ratio of 2.5:1.5 (mass ratio of sodium peroxide:sodium hydroxide), take 3 g of the above - mixed combined alkali flux and add it to the above - mentioned vessel and stir evenly. Then cover it with 1 g of the above - mentioned combined alkali flux. After covering the lid, place it in a muffle furnace pre - heated to 650 °C, heat it up to 700 °C and keep it for 5 min - 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0076] The measurement method steps are all detected in accordance with the national standard GB / T 14352.1—2010.

[0077] Examples 35 - 37

[0078] The difference from Comparative Examples 20 - 28 is only that: in the combined alkali flux used: the alkali flux uses a sodium peroxide / sodium hydroxide combined alkali flux.

[0079] That is, place the ore sample to be measured in a vessel (iron crucible or corundum crucible). After mixing the combined alkali flux (sodium peroxide and sodium hydroxide) evenly according to the mass ratio of 2:2 (mass ratio of sodium peroxide:sodium hydroxide), take 2 g of the above - mixed combined alkali flux and add it to the above - mentioned vessel and stir evenly. Then cover it with 2 g of the above - mentioned combined alkali flux. After covering the lid, place it in a muffle furnace pre - heated to 650 °C, heat it up to 700 °C and keep it for 5 min - 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0080] The measurement method steps are all detected in accordance with the national standard GB / T 14352.1—2010.

[0081] Examples 38 - 46

[0082] The difference from Comparative Examples 20 - 28 is only that: the alkali flux uses a sodium peroxide / sodium hydroxide combined alkali flux.

[0083] That is, place the ore sample to be tested in a vessel (iron crucible or corundum crucible). After mixing the combined alkali flux (sodium peroxide and sodium hydroxide) evenly according to the mass ratio of 2.8:1.2 (mass ratio of sodium peroxide to sodium hydroxide), take 3 g of the above-mentioned evenly mixed combined alkali flux and add it to the above-mentioned vessel and stir evenly. Then cover it with 1 g of the above-mentioned combined alkali flux. After covering the lid, place it in a muffle furnace preheated to 650 °C, heat it to 700 °C and keep it for 5 min to 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0084] The steps of the determination method are all detected in accordance with the national standard GB / T 14352.1—2010.

[0085] Table 8 Comparison of the results of melting ore samples with combined alkali fluxes in different combinations and all sodium peroxide alkali fluxes

[0086]

[0087] According to the data in Table 8 above, the analysis results of melting ore samples with combined alkali fluxes in different combinations and all sodium peroxide alkali fluxes are all within the allowable error range, and the degree of coincidence is relatively high. However, as the addition amount of sodium hydroxide in the combined alkali flux increases, the oxidation ability in the alkali flux becomes weaker, and the falling-off speed gradually slows down when extracting the 2% ethanol solution from the melted ore sample. It is significantly slower in Examples 26 - 34 and Examples 35 - 37. Combining the falling-off speed when extracting the ethanol solution from the melted ore sample with different ratios of combined agents and the analysis results of the ore samples, the mass ratio of sodium peroxide to sodium hydroxide in the combined agent is preferably 3:1 to 2.8:1.2. " / " in the above table indicates that the falling-off speed is slower when extracting the 2% ethanol solution from the ore sample after subsequent melting of this combination.

[0088] Comparative Examples 29 - 38

[0089] The difference from Comparative Examples 1 - 8 is only that: the tested samples are different.

[0090] Examples 47 - 56

[0091] The difference from Comparative Examples 29 - 38 is only that: the alkali flux uses a combined alkali flux of sodium peroxide / sodium hydroxide (mass ratio 2.8:1.2).

[0092] Specifically: Replace the single sodium peroxide alkali flux with a combined alkali flux of sodium peroxide / sodium hydroxide. Take 2.8 g of sodium peroxide and add it to the above-mentioned vessel and stir evenly. Then cover it with 1.2 g of sodium hydroxide. After covering the lid, place it in a muffle furnace preheated to 650 °C, heat it to 700 °C and keep it for 5 min to 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0093] The steps of the determination method are all detected in accordance with the national standard GB / T 14352.1—2010.

[0094] Examples 57 - 66

[0095] The differences from Comparative Examples 29 - 38 are only as follows: The differences from Comparative Examples 29 - 38 are only as follows: The alkali flux uses a combined alkali flux of sodium peroxide / sodium hydroxide (mass ratio 2.5:1.5). And the addition method of the combined alkali flux is different.

[0096] Specifically: Replace the single sodium peroxide alkali flux with the combined alkali flux of sodium peroxide / sodium hydroxide. Take 2.5 g of sodium peroxide and add it to the above-mentioned vessel and stir evenly, then cover it with 1.5 g of sodium hydroxide. After covering the lid, place it in a muffle furnace preheated to 650 °C, heat it up to 700 °C and keep it for 5 min - 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0097] The measurement method steps are all detected in accordance with the national standard GB / T 14352.1—2010.

[0098] Table 9 Verification process condition settings for melting ore samples with different addition methods of the combined agent in the vessel

[0099] Project Flux name Dosage Bottom + covering Set temperature for high-temperature melting Comparative examples 29 - 38 Sodium peroxide 4g All 700℃ Examples 47 - 56 Combined alkali flux 4g Multiple 700℃ Examples 57 - 66 Combined alkali flux 4g Multiple 700℃

[0100] Table 10 Result comparison of melting ore samples with different addition methods of the combined agent in the vessel

[0101]

[0102]

[0103] According to the analysis and comparison of the experimental results in Table 10, when using all sodium peroxide to melt the ore samples in Comparative Examples 29 - 38, it is easy to dissolve. When taking 2% ethanol solution, the molten minerals fall off quickly. In Examples 47 - 56, 2.8 g of sodium peroxide is used at the bottom and 1.2 g of sodium hydroxide is covered. The ore samples in the melting vessel are exposed and cannot be completely covered. When taking 2% ethanol solution, the melt falls off slightly slower and falls off completely after about 3 minutes. In Examples 47 - 56, 2.5 g of sodium peroxide is used at the bottom and 1.5 g of sodium hydroxide is covered. The ore samples in the melting vessel are exposed and cannot be completely covered. When taking 2% ethanol solution, the melt falls off slowly and it takes more than 3 minutes for it to fall off completely.

[0104] From the above result analysis, it can be seen that the addition methods of the combination agents with different combination ratios above in the melting vessel are different, and the analysis results are all within the allowable error range, with a high degree of coincidence. In Examples 47 - 56 and Examples 57 - 66, sodium hydroxide is separately covered on the upper part. When taking 2% ethanol solution, the shedding of the melt becomes slower. According to the above analysis results, the shedding speed of the melt when taking 2% ethanol solution, and the preparation process of the combination agent, through comprehensive analysis, the optimal ratio of the combination agent selected in Examples 1 - 8 is 3g of sodium peroxide + 1g of sodium hydroxide. Before use, the two combination agents are fully mixed according to the ratio. When melting the ore sample, 3g of the mixed combined alkali flux is added to the bottom of the vessel, and 1g of the mixed combined alkali flux is covered on the upper part, which has good feasibility.

[0105] Comparative Examples 39 - 46

[0106] The difference from Comparative Examples 1 - 8 is only that: the tested samples are different. In this comparative example, tailing ore samples are all tested.

[0107] Examples 67 - 74

[0108] The difference from Comparative Examples 39 - 46 is only that: the combined alkali flux of sodium peroxide / sodium hydroxide is used to replace the single sodium peroxide alkali flux, in which sodium peroxide and sodium hydroxide are uniformly mixed according to a mass ratio of 3:1. Take 3g of the combined alkali flux and add it to the above vessel and stir evenly, then cover 1g of the combined alkali flux, cover the lid, and place it in a high-temperature furnace preheated to 650°C, heat up to 700°C and keep it for 5 min - 7 min until the melt just shows a completely molten state. Take it out and cool slightly.

[0109] The steps of the determination method are all detected in accordance with the national standard GB / T 14352.1—2010.

[0110] Table 11 Comparison of analysis results of 3g sodium peroxide + 1g sodium hydroxide combined alkali flux and all sodium peroxide molten tailing samples

[0111] Project Flux name Dosage Bottom + covering Set temperature for high-temperature melting Comparative examples 39 - 46 Sodium peroxide 4g <![CDATA[All Na 2 O 2 > 700℃ Examples 67 - 74 Combined alkali flux 4g 3g + 1g 700℃

[0112] Table 12 Comparison of analysis results of molten tailing samples

[0113] Ore sample number <![CDATA[Total Na 2 O 2 (%)]]> Combined alkali flux (%) Difference 32# 0.0149 0.0151 -0.0002 33# 0.0151 0.0147 0.0004 34# 0.0174 0.0175 -0.0001 35# 0.0120 0.0118 -0.0002 36# 0.0150 0.0151 -0.0001 37# 0.0159 0.0147 0.0002 38# 0.167 0.164 0.0003 Average 0.0153 0.0150 0.0003

[0114] Stability verification of combined alkali flux

[0115] Comparative Example 47

[0116] The difference from Comparative Examples 1 - 8 is only that: the tested ore samples are different. In this comparative example, the same batch of ore samples are tested 6 times respectively to verify the stability of the test results.

[0117] Example 75

[0118] It is only different from Comparative Example 47 of the experiment in that: a combined alkali flux of sodium peroxide / sodium hydroxide is used to replace the single sodium peroxide alkali flux, wherein sodium peroxide and sodium hydroxide are mixed evenly at a mass ratio of 3:1. 3 g of the combined alkali flux is taken and added to the above-mentioned vessel and stirred evenly, and then 1 g of the combined alkali flux is covered. After covering the lid, it is placed in a high-temperature furnace preheated to 650 °C, heated to 700 °C and maintained for 5 min to 7 min until the melt just becomes completely molten. Take it out and let it cool slightly.

[0119] The steps of the measurement method are all detected in accordance with the national standard GB / T 14352.1—2010.

[0120] Table 13 Setting of stability verification conditions for the results of melting ore samples with a combined alkali flux

[0121] Item Flux name Dosage Bottom + covering Set temperature for high-temperature melting Comparative example 47 Sodium peroxide 4g <![CDATA[All Na 2 O 2 > 700℃ Example 75 Combined alkali flux 4g 3g + 1g 700℃

[0122] Table 14 Stability verification of the results of melting ore samples with all sodium peroxide in Comparative Example 47

[0123]

[0124]

[0125] Example 75 Stability verification of the results of melting ore samples with a combined alkali flux

[0126]

[0127] The above data shows that the use of a combined alkali flux to melt ore samples has no obvious difference in the influence on the stability of the analysis results compared with the use of sodium peroxide alone. Therefore, the results of melting ore samples with a combined alkali flux have good stability and meet the requirements of analysis and detection.

[0128] The above is only a preferred embodiment of the present invention, and does not impose any form of limitation on the present invention. Although the present invention has been disclosed above with preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some changes or modifications to equivalent embodiments by using the above-disclosed technical content within the scope of the technical solution of the present invention. However, as long as it does not depart from the content of the technical solution of the present invention, any simple modification, equivalent change and modification made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A novel combined alkali flux, characterized in that: The invention comprises sodium peroxide and sodium hydroxide, wherein the mass ratio of the sodium peroxide to the sodium hydroxide is 3.5:0.5-2.8:1.

2.

2. The novel combined alkali flux according to claim 1, characterized in that: The mass ratio of the sodium peroxide to the sodium hydroxide is 3:1 to 2.8:1.

2.

3. The novel combined alkali flux according to claim 1, characterized in that: The mass ratio of the sodium peroxide to the sodium hydroxide is 3:

1.

4. A chemical analysis method using the novel combined alkali flux according to claim 1 or 2, characterized in that: The tungsten content is determined by using the combined alkali flux and according to the method in the national standard GB / T 14352.1-2010.

5. A detection method for detecting tungsten trioxide combined alkali flux in molten ore sample according to claim 3, characterized in that: Place the ore sample to be tested in an iron crucible or a corundum crucible, mix the combined alkali flux evenly according to the above mass ratio, take the first mass of the combined alkali flux and add it to the above container and stir it evenly, then cover it with the second mass of the combined alkali flux, cover it, and place it in a pre-heated high-temperature furnace for melting.

6. A chemical analysis method using the novel combined alkali flux according to claim 5, characterized in that: The sum of the first mass and the second mass is 4 g, and the mass ratio of the first mass: the second mass is 3:1 to 2.5:1.

5.

7. A chemical analysis method using the novel combined alkali flux according to claim 5 or 6, characterized in that: Place the ore sample to be tested in an iron crucible or a corundum crucible, mix the combined alkali flux in a mass ratio of 3:1~2.8:1.2, take 3g of the combined alkali flux and add it to the above container and stir evenly, then cover it with 1g of the combined alkali flux, cover it, and place it in a high-temperature furnace that has been pre-heated to 650℃, heat it to 700℃ and keep it for 5 min~7 min until the melt is just fully melted.

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