Method for determining rhodium content in waste rhodium Park catalyst mother liquor

Abstract

The invention discloses a method for measuring the content of rhodium in waste rhodium Park catalyst mother liquor, and relates to the technical field of analysis and detection.The method comprises the steps that the waste rhodium Park catalyst mother liquor is added into an acidizing organic solvent to be diluted for the first time and diluted for the second time in sequence; and respectively measuring the rhodium content in the acidified organic solvent and the diluent diluted for the second time by adopting inductively coupled plasma mass spectrometry, subtracting the rhodium content test value of the acidified organic solvent, and converting to obtain the rhodium content in the waste rhodium Park catalyst mother liquor. The method disclosed by the invention is particularly suitable for determining the content of trace rhodium in the waste rhodium Park catalyst mother liquor, and has the characteristics of simplicity in operation, high test speed, accurate test result and environmental friendliness.

Description

Technical Field

[0001] The invention relates to the technical field of analysis and detection, and further to a method for determining the rhodium content in a waste rhodium Parker catalyst mother liquor. Background Art

[0002] Rhodium triphenylphosphine carbonyl acetylacetonate (ROPAC), also known as Rhodium Parker, is an industrial catalyst for the production of butyl octanol by low-pressure propylene carbonylation. With the extension of production time and the accumulation of poisons, its activity will gradually decrease until it is completely inactivated, and the scrapped catalyst and reaction liquid will form a recyclable mother liquor. Rhodium metal is expensive, and the accurate quantification of rhodium in the mother liquor of the waste Rhodium Parker catalyst and its scientific recovery have important social and economic significance.

[0003] The components of waste rhodium Parker catalyst are complex, containing rhodium complexes, butyraldehyde trimers and polymers, triphenylphosphine or triphenylphosphine oxide and other organic components. The rhodium content in waste rhodium Parker catalyst is low, and it contains highly volatile organic components and difficult-to-handle macromolecular organic matter, making it difficult to accurately measure the rhodium content.

[0004] In the prior art, the determination of rhodium in the mother liquor of waste rhodium Parker catalyst mainly involves pre-treating the sample to obtain an inorganic aqueous solution, and then detecting it using an inductively coupled plasma instrument, an atomic absorption spectrometer, etc. The main sample pre-treatment methods include burning method, electric hot plate digestion method, microwave digestion method, etc. During burning, part of the rhodium will volatilize with the flue gas and cause loss, resulting in low test results; the electric hot plate digestion method has cumbersome steps, is time-consuming, and has high work intensity. The most commonly used method is to use strong acids such as nitric acid and sulfuric acid and add hydrogen peroxide to perform microwave digestion on the sample. This method can better avoid the loss of rhodium elements, and the organic components can also be completely digested.

[0005] CN 105572104 A adopts heating evaporation at 50-100 degrees until there is no obvious overflow of steam to remove low-boiling point organic matter, then increases the heating temperature to 300-600 degrees to carbonize and decompose high-boiling point organic matter to obtain rhodium-containing black slag; maintains high temperature to add peroxide to the rhodium-containing black slag for roasting and melting; then dissolves the obtained mixture with hydrochloric acid solution, and after constant volume, uses ICP method to determine the rhodium content in the solution to accurately determine the rhodium content in the rhodium-containing organic solution. However, this method cannot guarantee the possible loss of rhodium element in the volatilization and carbonization decomposition process of low-boiling point organic matter, and the process of this method is complicated and will cause certain environmental pollution.

[0006] CN 115824767 A provides a digestion and determination method for rhodium octanoate mother liquor, and studies the problems of high organic content and difficulty in determining trace rhodium. The method has the characteristics of rapid digestion, complete decomposition, no volatilization loss of elements, low acid consumption, accurate detection results, simple operation, flexibility and high efficiency, and can determine trace rhodium at the ppm level. The method adopts a composite digestion system of nitric acid, hydrogen peroxide and hydrofluoric acid, and uses aqua regia and hydrochloric acid to drive out the acid in steps, which is a big problem for environmental protection.

[0007] CN 113125367 A provides a method for detecting rhodium in an aqueous solution. In order to effectively eliminate the influence of coexisting metal cations on rhodium determination in a water-soluble rhodium phosphine complex-catalyzed olefin hydroformylation reaction system, improve the sensitivity of the method, and eliminate interference, the method first uses a heating method to remove part of the low-boiling organic matter, and then uses concentrated sulfuric acid to heat and digest. After the digestion is completed, continue to heat, evaporate sulfuric acid to a nearly dry state, add concentrated nitric acid after cooling, and continue to heat until the solution becomes colorless and transparent. When using a flame atomic absorption spectrometer for testing, add 2mg / mL-12mg / mL of LaCl3 and 2mg / mL-15mg / mL of CuSO4. The method is lengthy and complicated and cannot guarantee the loss of rhodium element during sample preparation.

[0008] As we all know, in order to ensure safety, microwave digestion has strict requirements on the amount of organic samples, generally not exceeding 0.1g. As mentioned earlier, in addition to macromolecular organic substances such as butyraldehyde polymers and triphenylphosphine, the waste rhodium Parker catalyst mother liquor also contains volatile butyraldehyde, butanol and other low-molecular organic substances, which poses a huge challenge to the accurate measurement of samples weighing about 0.1g. Since the sample amount itself is small, it has a greater impact on the calculation of subsequent dilution multiples, which in turn seriously affects the final test data. In the actual weighing process, it was found that when the balance indication was stable, the weighing area was filled with a strong smell of aldehydes. Therefore, it is necessary to find a simple, fast, accurate, and environmentally friendly method for detecting the rhodium content in the waste rhodium catalyst mother liquor. Summary of the invention

[0009] In order to solve the problems existing in the prior art, the present invention provides a method for determining the rhodium content in waste rhodium Parker catalyst mother liquor. The method of the present invention has the characteristics of simple operation, fast test speed, accurate test results and environmental friendliness.

[0010] One of the objects of the present invention is to provide a method for determining the rhodium content in a waste rhodium Parker catalyst mother liquor.

[0011] A method for determining the rhodium content in waste rhodium Parker catalyst mother liquor, characterized in that the method comprises:

[0012] After the waste rhodium Parker catalyst mother liquor is added to the acidified organic solvent for the first dilution and the second dilution, the rhodium content in the acidified organic solvent as the blank solvent and the dilution liquid after the second dilution is respectively determined by inductively coupled plasma mass spectrometry, and the rhodium content in the waste rhodium Parker catalyst mother liquor is obtained by subtracting the rhodium content test value of the blank solvent. In particular, the inventors found in the experiment that using the acidified organic solvent to dilute the waste rhodium Parker catalyst mother liquor can obtain better test results.

[0013] Preferably,

[0014] The acidified organic solvent is a mixture of concentrated inorganic acid and an organic solvent; and / or,

[0015] The waste rhodium Parker catalyst mother liquor is a rhodium-containing waste catalyst solution produced by carbonylation reaction;

[0016] Preferably,

[0017] The waste rhodium Parker catalyst mother liquor is a rhodium-containing waste catalyst solution generated by producing butanol.

[0018] Preferably,

[0019] The concentration of the concentrated inorganic acid is 50wt%-75wt%; and / or,

[0020] The volume ratio of the concentrated inorganic acid to the organic solvent is (1-5):100.

[0021] Preferably,

[0022] The rhodium content in the waste rhodium Parker catalyst mother liquor is generally between 600-800 mg / Kg. Since the ICP-MS detection sensitivity is relatively high, the instrument detection range is set to be no more than 100 μg / Kg, so the sample needs to be diluted twice. After the second dilution of the waste rhodium Parker catalyst mother liquor of the present invention, the rhodium element concentration in the diluted solution is 0.5 μg / Kg-10 mg / Kg, preferably 1 μg / Kg-5 mg / Kg, and more preferably 10 μg / Kg-1 mg / Kg.

[0023] Preferably,

[0024] The first dilution uses 0.1-10 ml of waste rhodium Parker catalyst mother liquor, preferably 0.5-5 ml, more preferably 1-3 ml; and / or,

[0025] The volume ratio of the waste rhodium Parker catalyst mother liquor used in the first dilution to the acidified organic solvent is 1:(1-500), preferably 1:(10-100); and / or,

[0026] The diluent used in the second dilution after the first dilution is 0.01 to 10 ml, preferably 0.05 to 5 ml, more preferably 0.1 to 3 ml; and / or,

[0027] The volume ratio of the diluent after the first dilution used in the second dilution to the acidified organic solvent is 1:(1-1000), preferably 1:(10-500).

[0028] Preferably,

[0029] The concentrated inorganic acid is at least one of concentrated nitric acid, concentrated hydrochloric acid and concentrated sulfuric acid, preferably concentrated nitric acid, because concentrated nitric acid can effectively avoid interference from elements such as S / Cl in concentrated hydrochloric acid and concentrated sulfuric acid; and / or,

[0030] The organic solvent is at least one of ethanol, isopropanol, toluene, dimethyl sulfoxide, N-methylpyrrolidone, propylene glycol monomethyl ether, and propylene glycol methyl ether acetate, preferably N-methylpyrrolidone; and / or,

[0031] The organic solvent is of electronic grade, preferably of G2 grade or above.

[0032] Preferably,

[0033] The inductively coupled plasma mass spectrometer is equipped with an organic oxygen addition system.

[0034] Preferably,

[0035] The inductively coupled plasma mass spectrometer is equipped with a dynamic reaction cell system.

[0036] Preferably,

[0037] The reaction gas of the inductively coupled plasma mass spectrometer includes helium;

[0038] Preferably,

[0039] The reaction gas of the inductively coupled plasma mass spectrometer includes helium and other gases;

[0040] Preferably,

[0041] The other gas is argon or oxygen.

[0042] Preferably,

[0043] The purity of the reaction gas of the inductively coupled plasma mass spectrometer is not less than 99.99v%, preferably not less than 99.999v%.

[0044] Preferably,

[0045] The measurement conditions of the inductively coupled plasma mass spectrometry are: power 800 W; cold plasma lens; platinum sampling cone and intercepting cone; matrix tube depth: 10 mm; peristaltic pump speed: 20 rpm / min; atomization chamber temperature: -5°C; plasma cooling gas flow: 14 L / min; atomization gas flow: 0.67 L / min; auxiliary gas flow: 0.8 L / min; He gas flow: 4.5 mL / min; O2 flow: 37 mL / min; the gas flow is controlled by a precision flow meter.

[0046] The following solutions can be adopted:

[0047] 1) slowly adding concentrated inorganic acid to an organic solvent to prepare an acidified organic solvent with a volume ratio of concentrated inorganic acid to organic solvent of (1-5):100;

[0048] 2) taking 0.1-10 mL of waste rhodium Parker catalyst mother liquor and adding it into 0.1-5000 mL of acidified organic solvent for the first dilution;

[0049] 3) taking 0.01-10 mL of the dilution obtained in step 2), adding 0.01-10000 mL of an acidified organic solvent for secondary dilution;

[0050] 4) using ICP-MS to measure the rhodium content in the blank solvent and the dilution solution after secondary dilution;

[0051] 5) The rhodium content test value in the obtained dilution solution is subtracted from the test value of the rhodium content in the blank solvent, and the result is multiplied by the total dilution multiple to obtain the rhodium element content value in the waste rhodium Parker catalyst mother liquor.

[0052] Compared with the prior art, the present invention realizes the accurate determination of trace rhodium in waste rhodium Parker catalyst mother liquor only by solvent dilution method, and the operation is simple; the sample is dissolved in an acidified organic solvent, which minimizes the impact of the volatilization of volatile organic components; the whole test process has few operation steps, which reduces the probability of impurity introduction and loss of the measured element; during the test, the organic components in the sample are fully burned by the ICP-MS organic oxygenation mode, and the organic components are discharged after forming carbon dioxide and water, which is relatively environmentally friendly, and effectively reduces the interference of organic components on the measured elements, and realizes the method of directly injecting organic samples to determine the rhodium content; in particular, the use of acidified organic solvents can obtain better test results. The method of the present invention is particularly suitable for the determination of trace rhodium content in waste rhodium Parker catalyst mother liquor, and has the characteristics of simple operation, fast test speed, accurate test results, and environmental friendliness. BRIEF DESCRIPTION OF THE DRAWINGS

[0053] Figure 1 The standard addition method working curve of Example 1;

[0054] Figure 2 This is the external standard curve obtained by converting the standard addition method working curve of Example 1. DETAILED DESCRIPTION

[0055] The present invention is described in detail below in conjunction with specific drawings and embodiments. It is necessary to point out that the following embodiments are only used to further illustrate the present invention and cannot be understood as limiting the scope of protection of the present invention. Some non-essential improvements and adjustments made to the present invention by those skilled in the art based on the content of the present invention still fall within the scope of protection of the present invention.

[0056] The raw materials and reagents used in the examples and comparative examples of the present invention are all commercially available products, and the specific information is as follows:

[0057] Argon (≥99.99% (V / V)); oxygen (≥99.99% (V / V)); helium (≥99.99% (V / V)); rhodium standard solution (1000ug / ml, National Nonferrous Metals and Electronic Materials Analysis and Testing Center); isopropyl alcohol (Shanghai Aoban Technology Co., Ltd., G4, electronic grade, metal ion content ≤10ppt); N-methylpyrrolidone (Shanghai Aoban Technology Co., Ltd., G4, electronic grade, metal ion content ≤10ppt); propylene glycol monomethyl ether (Shanghai Aoban Technology Co., Ltd., G4, electronic grade, metal ion content ≤10ppt); concentrated nitric acid (Beijing Institute of Chemical Reagents, BV-III);

[0058] Equipment used:

[0059] Mettler electronic balance XP205, d = 0.01 mg; inductively coupled plasma mass spectrometer (Thermo Fisher iCAPTQ) (equipped with PFA microflow concentric nebulizer, oxygenation system controls O2 flow rate through precision flowmeter); PFA reagent bottle (Nanjing Binzhenghong Plastic Co., Ltd.);

[0060] Inductively coupled plasma mass spectrometer (ICP-MS) measurement conditions: power 800W; cold plasma lens; platinum sampling cone and interceptor cone; rectangular tube depth: 10mm; peristaltic pump speed: 20rpm / min; spray chamber temperature: -5℃; plasma cooling gas flow: 14L / min; spray gas flow: 0.67L / min; auxiliary gas flow: 0.8L / min; dynamic reaction cell system He gas flow: 4.5mL / min; oxygenation system O2 flow: 37mL / min;

[0061] All pipettes used were calibrated.

[0062] Sample dilution method:

[0063] The rhodium content in the waste rhodium Parker catalyst mother liquor is generally between 600-800 mg / Kg. The ICP-MS detection sensitivity is relatively high. The instrument detection range is set to no more than 100 μg / Kg, and the sample needs to be diluted twice.

[0064] A. Take a PFA reagent bottle, weigh it accurately with a balance, peel it, use a pipette to transfer 98mL of N-methylpyrrolidone into the PFA reagent bottle, then use a pipette to transfer 2mL of concentrated nitric acid into the PFA reagent bottle, shake well, and obtain acidified N-methylpyrrolidone. The concentration of nitric acid is 2% (v / v);

[0065] B. Take a PFA reagent bottle, weigh it accurately with a balance, peel it, use a pipette to transfer 40mL of acidified N-methylpyrrolidone into the PFA reagent bottle, use a balance to weigh it accurately, record it as m1, use a pipette to transfer 1mL of waste rhodium Parker catalyst mother liquor (rhodium-containing waste catalyst solution produced by the production of butyl octanol) into the PFA reagent bottle, shake well, weigh it, record it as m2;

[0066] C. Take another PFA reagent bottle, weigh it accurately with a balance, peel it, use a pipette to transfer 20mL of acidified N-methylpyrrolidone into the reagent bottle, use a balance to weigh it accurately, record it as m3, use a pipette to transfer 0.1mL of the solution prepared in step A into the reagent bottle, shake well, weigh it, record it as m4; this dilution is the zero-point solution of the standard addition method.

[0067] Drawing of the working curve of the standard addition method:

[0068] Under the working conditions of an inductively coupled plasma mass spectrometer (ICP-MS), the rhodium content in the acidified N-methylpyrrolidone is first determined as a blank value A0, and then the rhodium content in the zero-point solution of step C is determined. After the measurement, the solution is weighed, and an appropriate amount of rhodium standard solution is added, and the solution is weighed. The mass of the rhodium standard solution added is calculated according to the mass difference, and the mass of the rhodium element added to the solution is calculated. The concentration is taken as the first concentration point, and the rhodium content in the solution is determined on the machine; rhodium standard solutions of different concentrations are prepared and measured in turn, and a standard addition method working curve is drawn. The horizontal axis concentration corresponding to the vertical axis zero point is the concentration of the rhodium element in the secondary dilution solution, which is recorded as A. The working curve obtained in Example 1 is shown in the attached figure. Figure 1 , convert the standard addition method working curve into an external standard curve (attached Figure 2 ) can be used for quantitative analysis of rhodium in similar solutions of other matrices.

[0069] Calculation results:

[0070] Subtract the blank value from the A value and multiply it by the sample dilution factor to get the rhodium content in the sample. The specific calculation formula is as follows:

[0071] Rh content = (A-A0)*m4m2 / (m4-m3)(m2-m1) / 10 4

[0072] Rh content: trace rhodium content in waste rhodium Parker catalyst mother liquor, mg / Kg;

[0073] A: Rhodium content in the secondary dilution solution, μg / Kg;

[0074] A0: Rhodium content in acidified N-methylpyrrolidone, μg / Kg;

[0075] m1: the mass of 40 mL of acidified N-methylpyrrolidone taken for the first time, g;

[0076] m2: the total mass of 1 mL of spent rhodium Parker catalyst mother liquor and 40 mL of acidified N-methylpyrrolidone taken for the first time, g;

[0077] m3: the mass of 20 mL of acidified N-methylpyrrolidone removed for the second time, g;

[0078] m4: the total mass of 0.1 mL of the solution prepared in step A and 20 mL of acidified N-methylpyrrolidone taken the second time, g;

[0079] Example 1

[0080] 1) Take a PFA reagent bottle, weigh it accurately with a balance, peel it, use a pipette to transfer 40 mL of the above acidified N-methylpyrrolidone into the PFA reagent bottle, use a balance to accurately weigh it, the mass is 41.41668 g, use a pipette to transfer 1 mL of the waste rhodium Parker catalyst mother liquor into the PFA reagent bottle, shake well, weigh it, the mass is 42.16280 g;

[0081] 2) Take another PFA reagent bottle, weigh it accurately with a balance, peel it, and use a pipette to transfer 20 mL of the above acidified N-methylpyrrolidone into the reagent bottle. Use a balance to accurately weigh it, and the mass is 20.34345 g. Use a pipette to transfer 0.1 mL of the solution prepared in step 1) into the reagent bottle, shake well, weigh it, and record it as 20.44826 g. This dilution is the zero-point solution of the standard addition method.

[0082] 3) Prepare concentration points of 0, 25.90, 51.54, and 100.73 μg / Kg respectively according to the method for drawing a standard curve, and use ICP-MS to determine the concentrations of rhodium in the acidified N-methylpyrrolidone as a blank solution and the standard solution under working conditions, and draw a standard curve. The ICP-MS test shows that the rhodium content in the dilution is 75.17 μg / Kg, and the rhodium content in the sample is further calculated to be 859.6 mg / Kg.

[0083] Embodiment 2-6

[0084] The experimental steps are the same as those in Example 1, except that the samples are diluted by different multiples and measured using the marking line drawn in Example 1. The rhodium content in the samples is calculated and the results are shown in Table 1.

[0085] Table 1

[0086] Example Dilution multiple Test value / μg / Kg Results mg / Kg Example 2 11172.78 76.87 858.9 Example 3 11502.94 74.69 859.2 Example 4 22172.83 38.79 860.1 Example 5 23128.85 37.18 859.8 Example 6 22191.12 38.77 860.3

[0087] The sample of Example 6 was tested in step 3) four times in succession. The test results are shown in Table 2.

[0088] Table 2

[0089]

[0090] The sample of Example 6 was tested for spiked recovery: standard rhodium solutions with concentrations of 15.20 μg / Kg, 25.26 μg / Kg, 50.18 μg / Kg and 75.02 μg / Kg were added to the diluted solution of Example 6 diluted 22191.12 times, respectively. The recovery was calculated based on the test values ​​and the calculated values. The specific results are shown in Table 3.

[0091] Table 3

[0092] Added value / μg / Kg 15.20 25.26 50.18 75.02 Calculated value / μg / Kg 53.97 64.03 88.95 113.79 Test value / μg / Kg 54.25 64.85 88.21 113.18 Recovery rate / % 100.5 101.3 99.2 99.5

[0093] It can be seen from Table 3 that the recovery rate of the spiked rhodium element is between 99% and 102%, which can fully meet the requirements of quantitative testing.

[0094] Example 7

[0095] The experimental steps were the same as those in Example 1, except that N-methylpyrrolidone was replaced with isopropanol. The experimental results are shown in Table 4.

[0096] Example 8

[0097] The experimental steps were the same as those in Example 1, except that N-methyl 2-pyrrolidone was replaced with propylene glycol monomethyl ether. The experimental results are shown in Table 4.

[0098] Table 4

[0099] Example Results mg / Kg Example 7 842.6 Example 8 852.7

[0100] Comparative Example 1

[0101] The samples were digested by microwave and then the rhodium content in the samples was determined by ICP-MS.

[0102] 1) Use a pipette to transfer 100 μL of sample into a digestion tank, then add 8 mL of concentrated nitric acid and 2 mL of hydrogen peroxide respectively. Treat the sample and parallel samples under the same conditions and digest according to the following conditions and procedures;

[0103] The first step is to increase the temperature from room temperature to 100°C within 5 minutes and maintain it for 5 minutes; the second step is to increase the temperature from 100°C to 150°C within 5 minutes and maintain it for 5 minutes; the third step is to increase the temperature from 150°C to 180°C within 5 minutes and maintain it for 20 minutes.

[0104] 2) Prepare Rh standard solutions with concentrations of 0, 20, 40, and 80 μg / Kg using 2% nitric acid aqueous solution, and use In element with a concentration of 50 μg / Kg as an internal standard for calibration.

[0105] 3) Use ICP-MS to measure the standard solution and draw a standard curve.

[0106] 4) The samples were quantitatively analyzed and the calculation results are shown in Table 5.

[0107] Table 5

[0108]

[0109] It can be seen from the test results in Table 5 that the rhodium content measured after the samples were treated with microwave digestion was low and the RSD% value was high.

[0110] Comparative Example 2

[0111] The experimental steps were the same as those in Example 6, except that the acidified N-methylpyrrolidone was replaced with non-acidified N-methylpyrrolidone. The sample was tested in step 3) four times in succession. The test results are shown in Table 6.

[0112] Table 6

[0113]

[0114] It can be seen from the test results in Table 6 that compared with the repeated test results of Example 6 (Table 2), the RSD% of the rhodium element test using acidified N-methylpyrrolidone as the dilution solvent is lower, indicating that the use of acidified organic solvents for testing can achieve better test results.

Claims

1. A method for determining the rhodium content in waste rhodium Parker catalyst mother liquor, characterized in that The method comprises: The waste rhodium Parker catalyst mother liquor is added to an acidified organic solvent for the first dilution and the second dilution, and the rhodium content in the acidified organic solvent and the diluted liquid after the second dilution is determined by inductively coupled plasma mass spectrometry. After subtracting the test value of the rhodium content in the acidified organic solvent, the rhodium content in the waste rhodium Parker catalyst mother liquor is converted.

2. The method for measuring rhodium content in waste rhodium Parker catalyst mother liquor according to claim 1, characterized in that: The acidified organic solvent is a mixture of concentrated inorganic acid and an organic solvent; and / or, The waste rhodium Parker catalyst mother liquor is a rhodium-containing waste catalyst solution produced by carbonylation reaction; Preferably, The waste rhodium Parker catalyst mother liquor is a rhodium-containing waste catalyst solution generated by producing butanol.

3. The method for measuring the rhodium content in the waste rhodium Parker catalyst mother liquor according to claim 2, characterized in that: The concentration of the concentrated inorganic acid is 50wt%-75wt%; and / or, The volume ratio of the concentrated inorganic acid to the organic solvent is (1-5):

100.

4. The method for measuring rhodium content in waste rhodium Parker catalyst mother liquor according to claim 1, characterized in that: The first dilution uses 0.1-10 ml of waste rhodium Parker catalyst mother liquor, preferably 0.5-5 ml, more preferably 1-3 ml; and / or, The volume ratio of the waste rhodium Parker catalyst mother liquor used in the first dilution to the acidified organic solvent is 1:(1-500), preferably 1:(10-100); and / or, The diluent used in the second dilution is 0.01 to 10 ml, preferably 0.05 to 5 ml, more preferably 0.1 to 3 ml after the first dilution; and / or, The volume ratio of the diluent after the first dilution used in the second dilution to the acidified organic solvent is 1:(1-1000), preferably 1:(10-500).

5. The method for measuring rhodium content in waste rhodium Parker catalyst mother liquor according to claim 1, characterized in that: The concentrated inorganic acid is at least one of concentrated nitric acid, concentrated hydrochloric acid and concentrated sulfuric acid, preferably concentrated nitric acid; and / or, The organic solvent is at least one of ethanol, isopropanol, toluene, dimethyl sulfoxide, N-methylpyrrolidone, propylene glycol monomethyl ether, and propylene glycol methyl ether acetate, preferably N-methylpyrrolidone; and / or, The organic solvent is of electronic grade, preferably of G2 grade or above.

6. The method for measuring the rhodium content in the waste rhodium Parker catalyst mother liquor according to claim 1, characterized in that: The inductively coupled plasma mass spectrometer is equipped with an organic oxygen addition system.

7. The method for measuring the rhodium content in the waste rhodium Parker catalyst mother liquor according to claim 1, characterized in that: The inductively coupled plasma mass spectrometer is equipped with a dynamic reaction cell system.

8. The method for measuring the rhodium content in the waste rhodium Parker catalyst mother liquor according to claim 1, characterized in that: The reaction gas of the inductively coupled plasma mass spectrometer includes helium; Preferably, The reaction gas of the inductively coupled plasma mass spectrometer includes helium and other gases; Preferably, The other gas is argon or oxygen.

9. The method for measuring the rhodium content in the waste rhodium Parker catalyst mother liquor according to claim 1, characterized in that: The purity of the reaction gas of the inductively coupled plasma mass spectrometer is not less than 99.99v%, preferably not less than 99.999v%.

10. The method for measuring the rhodium content in the waste rhodium Parker catalyst mother liquor according to claim 1, characterized in that: The measurement conditions of the inductively coupled plasma mass spectrometry are: power 800W; cold plasma lens; Platinum sampling cone and intercepting cone; rectangular tube depth: 10mm; peristaltic pump speed: 20rpm / min; spray chamber temperature: -5℃; plasma cooling gas flow: 14L / min; nebulizing gas flow: 0.67L / min; auxiliary gas flow: 0.8L / min; He gas flow: 4.5mL / min; O2 flow: 37mL / min.

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