CN101526478B - Method for detecting bullion content of metal carrier catalytic converter - Google Patents
Method for detecting bullion content of metal carrier catalytic converter Download PDFInfo
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- CN101526478B CN101526478B CN2009101032047A CN200910103204A CN101526478B CN 101526478 B CN101526478 B CN 101526478B CN 2009101032047 A CN2009101032047 A CN 2009101032047A CN 200910103204 A CN200910103204 A CN 200910103204A CN 101526478 B CN101526478 B CN 101526478B
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Abstract
A method for detecting bullion content of a metal carrier catalytic converter comprises the following steps: soaking and heating the catalytic converter in HNO_3-HCl and boiling the catalytic converter for a while so as to facilitate coating with the noble metal to fall off the metal carrier easily; then, vibrating and cleaning the coating from the metal carrier in an ultrasonic clearing machine, collecting and evaporating to dryness the mixed liquor in the process of falling off of the coating and the mixed liquor in the process of cleaning; grinding, sampling, counteracting, dispensing and setting constant volume of the powder; using ICP to test bullion content, thus calculating the total content and ratio of the noble metal in the whole catalytic converter. The invention makes up for the gap of the method for testing bullion content in the metal carrier catalytic converter and features relatively small detection error in bullion content, easy operation and relatively low cost.
Description
Technical field
The present invention relates to the method for testing of bullion content on a kind of metallic carrier, particularly relate to the method for testing of the bullion content of metal carrier catalytic converter that uses on a kind of motorcycle.
Technical background
Catalytic converter is as the vitals that reduces motorcycle emission, and the use on motorcycle more and more widely.In catalytic converter, what play catalytic action is noble metal, so the ratio of noble metal and coating amount and car load emission compliance have confidential relation.Simultaneously, as one of key component in the auto exhaust after-treatment device, the extensive application of catalytic converter has aggravated the demand to noble metal platinum (Pt), palladium (Pd), rhodium (Rh), feasible deficient originally noble metal resource worsening shortages, noble metal price continuous rise causes the cost of raw material of catalyst converter to sharp rise.But, as motor depot, introducing and buying in the process of catalytic converter, because the shortage of equipment and laboratory facilities, especially the content and the ratio of noble metal all can't be controlled and be verified to the quality of catalytic converter.This is difficult to the content of noble metal in the catalytic converter and the consistance control of ratio, causes emission result that very big uncertainty is arranged.
1. the substantial connection of noble metal ratio and coating amount and car load emission compliance
In the reply process of state III rules, catalytic converter is as the main parts of machine after purification, its in the reply process of state III rules, the catalytic activity of its noble metal uniqueness, selectivity and stability, making it has irreplaceable direct effect in the performance of catalyst performance.Fig. 1 is the membership credentials figure of noble metal ratio and coating amount and car load emission compliance.Can find out intuitively that by this figure catalyst converter plays crucial effects for the car load emission control, and noble metal ratio and coating amount play a part to the catalytic purification performance of catalyst converter very important.
The product quality management of standard vehicle catalyst is a new car, in powerful measure with the car emission control, help standard catalyst converter market order simultaneously, promote applying of advanced technology and product.Department of China government concerned, industry organization and enterprise have given this to show great attention to.In GB14622-2007 " motorcycle pollutant emission limit instrumentation metering method (operating condition method, Chinese III stage) ", the content and the noble metal ratio of noble metal in the catalytic converter have also been made clear and definite regulation.Yet domestic detectability to noble metal is but extremely limited at present.
2. the price pressure of noble metal
Along with the fast development of world car industry and the progressively reinforcement of Abgasgesetz, the auto exhaust post-processing technology is progressively promoted.As one of key component in the auto exhaust after-treatment device, the extensive application of catalytic converter has aggravated the demand to noble metal platinum (Pt), palladium (Pd), rhodium (Rh), feasible deficient originally noble metal resource worsening shortages, noble metal price continuous rise causes the cost of raw material of catalyst converter to sharp rise.As Fig. 2 is the price trend of noble metal platinum and palladium over past ten years.
As can be seen from Figure 2: the price of platinum, was raising up again though the price of palladium descended before 10 years to some extent in recent years always at continuous rise in recent years.The second half year in 08 year, the noble metal price significantly decreased, and this mainly is the influence of financial crisis, and the depressed demand of noble metal that causes of international automobile industry descends price drops.But afterwards, the recovery of international automobile industry will cause the surging of noble metal price.
Meanwhile, car load/machine selling market has progressed into the maturity stage, and car load/machine price significantly glides, and car load/machine supplier's part price pressure has also been transferred to (the equal about 5-10% of catalyst converter year price rate of descent) on catalyst converter supplier's the body very naturally.Influenced on both side by this, catalyst converter supplier can only be helpless comes cost squeeze (noble metal cost account for whole catalyst converter cost about 60%) with the method that reduces noble metal dosage.Yet,, can guarantee that again the catalyst formulation of excellent activity and permanance and preparation technology's improvement way are unpractical simultaneously if think just to work out in a short time to reduce the noble metal use amount from the angle of technology.Point out among the CVEC " report of 2006 Motor Vehicle Pollution Prevention industry developments " that indivedual enterprises " after the car load authentication is finished, select some relatively poor catalyst converter starting material for use; Perhaps after car load has been produced a period of time, change the bullion content of carrier and minimizing catalyzer." according to the result of market study, the selling price of really more existing at present new car match and accessory catalyst converter even be lower than the noble metal cost illustrates that applying noble metal less even is not coated with, private changes phenomenon such as noble metal ratio and exists in the vehicle catalyst industry.This not only influences the consistance of new car catalytic converter, and has destroyed industry fair play order, has damaged the just and sincere of industry, has weakened the competitive strength of sincere enterprise, has hit the confidence of their sincerity operation.This report is pointed out " along with the development of technology; developed the instrument that can test bullion content in the ternary catalyzing unit abroad " again, " can often spot-check bullion content in the car catalyst converter;, cause reduction of catalyst converter transformation efficiency or mission life significantly to shorten " in case depot ' gives short weight ' in order to fall cost.
3. the scarcity of domestic bullion content of metal carrier catalytic converter method of testing
At present, domestic car load factory and encapsulation factory are very high to the demand of catalyst converter sampling check for quality, but the detectability of bullion content (chemical analysis method that comprises pre-treating method and bullion content) has only some big Catalyst Production manufacturers to possess, especially to motorcycle metallic carrier catalytic converter, also do not have effective method to prepare and detect the content and the ratio of noble metal.Though have a lot of colleges and universities or scientific research institution to possess the checkout equipment and the test capability of constituent content analysis, all lack pre-treatment ability (comprise the noble coatings desorption and clear up specimen preparation solution) to the metallic carrier catalyst converter.The check of bullion content is the approach to a quickness and high efficiency of the key component catalytic converter quality rapid screening in the exhaust aftertreatment devices.Recognized this point just, in order to seek the method for testing of metallic carrier catalytic converter noble metal, through exploration for a long time, creationary finally the invention can be with the coating that the contains noble metal method of desorption easily from the metallic carrier.After this method is found and grasped, can provide the coherence method of internal soundness control on the one hand for catalyzer enterprise; On the other hand, can also provide a convenient feasible approach (, can adopt existing national standard and environment-friendly products technical conditions to do further to judge for the rapid screening of catalyst converter for doubtful defective catalyst converter.)。Thus, can help the catalyzer industry to develop, guarantee that car load/machine discharges conformity of production and carries out smoothly to the standardization direction.
In the method for bullion content and ratio test, existing technological means mainly is at ceramic monolith.The method that the measurement of the catalytic converter noble metal of ceramic monolith is mainly used has: hydrometallurgy process, dry process process and dried hydrometallurgy process.Detection method mainly comprises three parts: specimen preparation, test solution preparation and analysis.Specimen preparation adopts full the pulverizing with machinery of sample to divide the sample abrasive method, with homogeneity and the representativeness of guaranteeing to take a sample; Test solution prepares the method that adopts the full decomposition of hydrochloric acid-nitric acid-hydrofluorite-perchloric acid, thoroughly destroys the lattice of metal oxide in the sample, makes the element to be measured in the sample all enter into test solution; Inductively coupled plasma atomic emission spectrometer is introduced in the test solution analysis, under selected optimal spectrum condition, measures the content of noble metal in the test solution.
But for the catalytic converter of metallic carrier, the detection method of above-mentioned bullion content is not easy to realize that this is mainly reflected in very much:
1, the pulverizing of metallic carrier, grinding ratio are difficult, are not easy to obtain uniform sample powder, branch sample unevenness is increased, thereby increased test errors;
2, the solubility of metallic carrier is bigger than ceramic monolith, and to causing difficulty separating of noble metal and metal, the interference to the test of noble metal also increases in the icp analysis process like this, makes test result more inaccurate.
Summary of the invention
The object of the present invention is to provide a kind of method of testing of bullion content of metal carrier catalytic converter, be intended to use straightforward procedure, coating on metallic carrier catalytic converter desorption from the metallic carrier is got off, by evaporate to dryness, grind, clear up, catch up with acid, process such as clear up, make solution to be analyzed, carry out the measurement of bullion content and ratio.On the one hand can be used to predict the efficient of catalyzed conversion, can verify the content and the ratio of noble metal in the catalyzer that catalytic converter producer reported on the other hand, provide foundation, the consistance of control catalytic converter the purchase and the use of catalytic converter.
Purpose of the present invention can reach by following technical measures, it is the method for testing of this bullion content of metal carrier catalytic converter, it is characterized in that: its uses contrary chloroazotic acid that the desorption from the metallic carrier of the coating that contains noble metal on the metallic carrier catalytic converter is got off, the metallic carrier catalytic converter is immersed in the contrary chloroazotic acid, be heated to fluidized state, keep whole catalytic converter to be immersed in the acid solution of boiling 2-3 hour; The coated powder hydrofluorite that will contain noble metal then, concentrated hydrochloric acid, the volume ratio of the mixed acid solution of perchloric acid and red fuming nitric acid (RFNA) and deionized water and chloroazotic acid be 1: 1 chloroazotic acid carry out two the step clear up, said digestion process is divided into two processes, first digestion process is to be hydrofluorite with volume ratio: concentrated hydrochloric acid: perchloric acid: red fuming nitric acid (RFNA)=6: 6: 1: 4 acid mixture will contain the coated powder submergence of noble metal, and be heated to the 110-130 degree and kept one hour, the interpolation of acid is red fuming nitric acid (RFNA) in proper order, perchloric acid, hydrochloric acid and hydrofluorite, be placed on after clearing up and be heated to the 130-150 degree on the electric furnace, acid no tangible liquid residue to the crucible is caught up with in acid solution evaporation, be the bulk solids of thickness; Second digestion process is that the volume ratio of will catch up with solid after the acid to add deionized water and chloroazotic acid is behind 1: 1 the chloroazotic acid, to be heated to the 120-140 degree and to clear up 20-40 minute on electric furnace, obtains not having muddy transparency liquid in crucible; Use the content of noble metal in the ICP instrument test sample at last.
Used contrary chloroazotic acid is that the volume ratio of a kind of red fuming nitric acid (RFNA) and concentrated hydrochloric acid is 3: 1 a mixed acid solution.
In the process of desorption, the assurance acid solution always can be flooded whole catalytic converter, and guarantees that acid solution is in fluidized state 2-3 hour always.
In order to reduce the interference of other ion pair testing process, whole clear up and the solution process for preparation in use deionized water to come clean container.
Use rare nitric acid of 5mol/L to come constant volume in the constant volume process.Its effect mainly is the precipitation that prevents noble metal, and behind constant volume that volumetric flask is airtight, prevents that the nitric acid volatilization from causing the noble metal precipitation.
The invention has the advantages that: can be with the coating that contains noble metal desorption and collecting from the metallic carrier more completely, the bullion content that can test metallic carrier catalytic converter bulk sample has higher accuracy; And in the process of desorption, can not destroy metallic carrier, reduced the influence of metallic ion to the noble metal test result.The method is simple to operate, convenient, error is little, is the new breakthrough of bullion content of metal carrier catalytic converter method of testing, has filled up the blank of domestic bullion content of metal carrier catalytic converter method of testing.For the bullion content of the catalytic converter of metallic carrier and the test of ratio provide a kind of simple but effective method.
Description of drawings
Fig. 1 is the membership credentials figure of noble metal ratio and coating amount and car load emission compliance;
Fig. 2 is the price trend figure of noble metal platinum and palladium over past ten years.
Embodiment
The method of testing of a kind of bullion content of metal carrier catalytic converter of the present invention, embodiment such as following:
1, pre-service
2 catalytic converter exemplars are numbered 1#, 2# respectively, and blank exemplar is 3#, and blank carrier is 4#
The teflon crucible is numbered 1#, 2#, 3# respectively
4 600ml beakers are numbered 1#, 2#, 3#, 4# respectively
4 600ml beakers be will remain and 1##, 2##, 3##, 4## will be numbered respectively
The 100ml volumetric flask is numbered 1#, 2#, 3# respectively
1#, 2# catalytic converter and blank exemplar 3#, blank carrier 4# are put into 110 ℃ of baking ovens dry to constant weight and weigh, weight is designated as W1-W4 respectively.
2, take off coat
1. measure red fuming nitric acid (RFNA) 1800ml at twice with the 1000ml graduated cylinder and pack in the 3000ml beaker, measure the 600ml concentrated hydrochloric acid again and join in the 3000ml beaker and mix, standby.
2. in the 1#-4# beaker, add the 1. middle complex acid solution 500ml of institute of step respectively with the 1000ml graduated cylinder, 1# after weighing, 2# catalytic converter and blank exemplar 3#, blank carrier 4# clamped with crucible tongs slowly put into corresponding 1#-4# beaker, add again part steps 1. in acid solution until catalytic converter is flooded fully.
3. the 1#-4# beaker is placed on and opens heating on the electric furnace, temperature is controlled at and just makes acid solution boiling (attention prevents that acid solution from spilling), and the beaker mouth covers to reduce the evaporation of acid solution, heated and boiled 2 hours with surface plate.
4. take out 1#-3# catalytic converter and 4# carrier in the 1##-4## beaker of putting into correspondence with crucible tongs after in the 1##-4## beaker, adding about 500ml high purity deionized water respectively, the 1##-4## beaker put in the ultrasonic cleaner cleaned about 10 minutes, with crucible tongs 1#-3# catalytic converter tune is cleaned during this time and guarantee for several times the coat all powder shaken and fall within the beaker and (then it is put back to if can not shake fully and continue heating half an hour in the corresponding former beaker, repeating step 4., until dropping fully).
5. put into baking oven after the 1#-4# catalytic converter substrates being dried up with air compressor machine and dry to constant weight and weigh in 110 ℃, weight is designated as W1 '-W4 ' respectively.
6. the surface plate of 1#-3# beaker mouth is opened, catch up with acid after remain the bulk solids in 220 ℃ solution in the beaker on electric furnace, treating that it takes off after the cooling solution in the 1##-3## beaker poured into continues to catch up with acid to the bulk solids that remains thickness in the corresponding 1#-3# beaker.
7. the 1#-3# beaker is put into baking oven and dried to constant weight in 110 ℃, take out the part solids and put into the mortar porphyrize, obtain powder.
3, Specimen eliminating
1. accurately take by weighing the powder 0.2000g that 7. step obtain and put into corresponding 1#-3# teflon crucible respectively.
2. in the 1#-3# crucible, add 12ml hydrofluorite, 12ml concentrated hydrochloric acid, 2ml perchloric acid, 8ml red fuming nitric acid (RFNA) (not having the sequence requirement of interpolation) respectively with transfer pipet, it is positioned on the electric boiling plate, close and be placed on 120 ℃ and clear up about 1 hour.
3. open teflon crucible lid, on heating plate, sample in the crucible is caught up with acid no tangible liquid residue to the crucible in 140 ℃, be the bulk solids of thickness.
4. in the 1#-3# crucible, add concentrated hydrochloric acid respectively: red fuming nitric acid (RFNA): behind the solution 30ml of water=3: 1: 4, close and be placed on 120 ℃ and clear up about 30 minutes, in crucible, obtain not having muddy transparency liquid.
5. prepare red fuming nitric acid (RFNA): the dilute nitric acid solution 300ml of high purity deionized water=1: 2 is standby, with dilute nitric acid solution drip wash one time of 1#-3# volumetric flask, transfer to liquid in the cooled 1#-3# crucible in the corresponding 1#-3# volumetric flask back with the careful drip wash 1#-3# crucible of dilute nitric acid solution, and the solution of drip wash also poured in the corresponding volumetric flask, so repeat several times up in crucible the liquid drip wash clean till (following on a small quantity repeatedly principle), with dilute nitric acid solution difference constant volume, shake up sample presentation again.
4, ICP test: undertaken by the associative operation rules, ratio and the proportionate relationship between the coated weight with test result during according to dosing are carried out inverse, thereby calculate total body burden of noble metal on the whole metallic carrier catalytic converter.
Claims (5)
1. the method for testing of a bullion content of metal carrier catalytic converter, it is characterized in that: its uses contrary chloroazotic acid that the desorption from the metallic carrier of the coating that contains noble metal on the metallic carrier catalytic converter is got off, this desorption is meant the metallic carrier catalytic converter is immersed in the contrary chloroazotic acid, be heated to fluidized state, keep whole catalytic converter to be immersed in the acid solution of boiling 2-3 hour; The coated powder hydrofluorite that will contain noble metal then, concentrated hydrochloric acid, the volume ratio of the mixed acid solution of perchloric acid and red fuming nitric acid (RFNA) and deionized water and chloroazotic acid is that 1: 1 chloroazotic acid carries out two step digestion process, first digestion process is to be hydrofluorite with volume ratio: concentrated hydrochloric acid: perchloric acid: red fuming nitric acid (RFNA)=6: 6: 1: 4 acid mixture will contain the coated powder submergence of noble metal, and be heated to the 110-130 degree and kept one hour, the interpolation of acid is red fuming nitric acid (RFNA) in proper order, perchloric acid, hydrochloric acid and hydrofluorite, be placed on after clearing up and be heated to the 130-150 degree on the electric furnace, acid no tangible liquid residue to the crucible is caught up with in acid solution evaporation, be the bulk solids of thickness; Second digestion process is that the volume ratio of will catch up with solid after the acid to add deionized water and chloroazotic acid is behind 1: 1 the chloroazotic acid, to be heated to the 120-140 degree and to clear up 20-40 minute on electric furnace, obtains not having muddy transparency liquid in crucible; Use the content of noble metal in the ICP instrument test sample at last.
2. the method for testing of bullion content of metal carrier catalytic converter according to claim 1, it is characterized in that: used contrary chloroazotic acid is that the volume ratio of a kind of red fuming nitric acid (RFNA) and concentrated hydrochloric acid is 3: 1 a mixed acid solution.
3. the method for testing of bullion content of metal carrier catalytic converter according to claim 1 is characterized in that: in the process of desorption, guarantee that acid solution always can flood whole catalytic converter, and guarantee that acid solution is in fluidized state 2-3 hour always.
4. the method for testing of bullion content of metal carrier catalytic converter according to claim 1 is characterized in that: in order to reduce the interference of other ion pair testing process, whole clear up and the solution process for preparation in use deionized water to come clean container.
5. the method for testing of bullion content of metal carrier catalytic converter according to claim 1, it is characterized in that: use rare nitric acid of 5mol/L to come constant volume in the constant volume process, its effect mainly is the precipitation that prevents noble metal, and behind constant volume that volumetric flask is airtight, prevent that the nitric acid volatilization from causing the noble metal precipitation.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101032047A CN101526478B (en) | 2009-02-17 | 2009-02-17 | Method for detecting bullion content of metal carrier catalytic converter |
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| CN2009101032047A CN101526478B (en) | 2009-02-17 | 2009-02-17 | Method for detecting bullion content of metal carrier catalytic converter |
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| CN101526478B true CN101526478B (en) | 2011-09-28 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2013539050A (en) * | 2010-10-08 | 2013-10-17 | ビーエーエスエフ ソシエタス・ヨーロピア | Analytical method for precious metals |
| CN102507364B (en) * | 2011-10-27 | 2014-03-05 | 四川中自尾气净化有限公司 | Surface coating deadsorbing and content determining method for catalytic converter |
| CN107037037A (en) * | 2017-03-16 | 2017-08-11 | 贵研铂业股份有限公司 | A kind of method of bullion content in ICP AES Accurate Determining solution |
| CN107063835A (en) * | 2017-03-29 | 2017-08-18 | 中国汽车技术研究中心 | The detection method of the digestion procedure of noble metal and precious metal element content in a kind of automobile-used ceramic catalytic converter |
| CN112284854A (en) * | 2020-10-28 | 2021-01-29 | 中汽研汽车检验中心（天津）有限公司 | Pretreatment method for determining content of noble metal in vehicle catalyst |
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Effective date of registration: 20180918 Address after: 402760 111 Yongjia Avenue, Bi Quan street, Bishan District, Chongqing. Patentee after: Chongqing Jialing Industrial Co., Ltd. Address before: 400032 Chongqing Shapingba District double monument 2301 mail box Patentee before: China Jialing Industry Co., Ltd. (Group) |
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