CN101446556B - Method for determining the platinum content in the catalytic reforming catalysts through the micro-wave digestion ICP method - Google Patents
Method for determining the platinum content in the catalytic reforming catalysts through the micro-wave digestion ICP method Download PDFInfo
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Abstract
A method for determining the platinum content in the catalysts through the micro-wave digestion ICP method, comprises, weighing dry sample of 0. 05-0. 2g in the micro-wave digestion jar, adding secondary deionized water wetting sample, aqua regia, and a cover, inserting in a protective sleeve and disposing secure spring leaf, pressing the jar tightly, preparing black sample, and then disposing and starting a micro-wave digestion instrument, setting the programme as, pressure of 25-40bar, and power of 300-700W, and the temperature rising programme as, rising to 200-200 DEG C for 5-10min, keeping the temperature for 25-40min, cooling, ending the digestion programme, taking out the jar, adding acid solution of about 2ml, fixing the volume as 10ml, and establishing the analysis method of the sample according to the working condition of ICP. The invention is capable of reducing the original sample processing time from 1-1. 5 day to 3-4 hours, only using acid solution of 7-10ml, to save determining cost, reduce the pollution to environment, and harm to human; and is featured with simple sample processing procedure without adding FeCl3 solution to avoid error and increase the accuracy ofthe determination.
Description
Technical field
The present invention relates to Al
2O
3Making the microwave treatment technology of the catalyst analysis sample of carrier, specifically, is the assay method of the ICP of metal platinum content in a kind of catalyzer.
Background technology
At the mensuration of metal platinum, generally all adopt chloroazotic acid during sample preparation, but the carrier A l of catalyzer
2O
3Use general sampler-dissolving method and but be difficult to dissolving fully, need constantly add chloroazotic acid, heating, length consuming time, solvent load is big and sample is difficult for thoroughly dissolving, easily causes the blank value height, pollutes problems such as big and element loss, the accuracy of influence experiment.The sample preparation link is " bottleneck " of the whole assay method of restriction all the time.
Liu Ying etc. are at " the useless Al of ICP-AES mensuration
2O
3Pt, Pd in catalyst based " describe in the article, take by weighing 0.5 gram and mix levigate sample to 100 orders, place 100 milliliters beaker.Add 5 milliliters of chloroazotic acid, be heated near doing under the proper temperature, and repeat 3 times, catch up with nitric acid, keep HCl (5+95) HCl acidity at last with hydrochloric acid; Or add 5 milliliters of sulfuric acid, and be heated to sample and dissolve fully, in 100 milliliters of volumetric flask constant volumes, on ICP-AES, measure.The acid solution consumption is big in its sample preparation, successively adds 5 milliliters of * 4=20 of chloroazotic acid milliliter for totally 4 times, adds 5 milliliters of sulfuric acid again, 25 milliliters of shared acid solutions; Moreover the sample preparation time is long, add 5 milliliters of chloroazotic acid earlier and be heated near doing, need 1-2 hour approximately, add 35 milliliters of chloroazotic acid again and be heated near doing, front and back need 5-8 hour altogether, and sample at this moment is dissolving fully not, adding 5 milliliters of sulfuric acid again is heated to sample and dissolves fully, also need about 1 hour, the time that sample grinds in addition, test is prepared, sample preparation needs 1-1.5 days approximately; Drawbacks such as test procedure is loaded down with trivial details in addition, staff's labour intensity is big, environmental pollution and experimentation cost height.
Jin Shan describes in " tin of low content in air-hydrogen flame aas determination reforming catalyst ": reforming catalyst is placed porcelain crucible, 850 ℃ of following calcinations of high temperature furnace 1 hour, take by weighing 0.5 gram sample after taking out cooling, place Pressure solution bullet, add 5 milliliters of concentrated hydrochloric acids, sealing back in 140 ± 10 ℃ of following constant temperature 4 hours, is taken out cooling and is changed in 50 milliliters of volumetric flasks in constant temperature oven, adds 2 milliliters of FeCl
3Solution with watery hydrochloric acid washing sample cup for several times, is settled to scale.Adopt the content of aas determination metallic tin, spectrum disturbs more, and the author has adopted the FeCl that adds 400ug/ml
3Solution is eliminated interference, makes test become loaded down with trivial details, introduces error easily; The sample preparation time is long, high temperature sintering 1 hour, the sample cooling needs about 3-4 hour, sample constant temperature 4 hours in the Pressure solution bullet constant temperature oven, cooling needs 2-3 hour, and Pressure solution bullet must cool off fully, when reducing to normal pressure, can open pressure, otherwise very dangerous, the sample preparation time needs 1.5 days at least like this, and the time is longer.
Aspect detection means, inductively coupled plasma (ICP) emission spectrometer is since 1975 come out, advantage such as just low because of its detectability, that precision is high, the mensuration range of linearity of concentration is wide, the phase mutual interference between the sample composition is little becomes the incomparable a kind of analysis means of other analytical technology aspect the mensuration simultaneously at trace element.
Summary of the invention
The method of Liu Ying etc. has drawbacks such as big, the consuming time length of sample preparation solvent load, test procedure is loaded down with trivial details in the prior art; Though the consumption of the method solvent of Jin Shan is not very big, have the dangerous height and the many drawbacks of atomic absorption spectrum test interference element of sample preparation length consuming time, complex steps and high-temperature operation, Pressure solution bullet.And the invention solves above-mentioned drawback, provide a kind of sample preparation time short, solvent load is few, hazard level is low and test the assay method of tenor in this catalyzer of noiseless element.
Technical scheme of the present invention is as follows
A kind of micro-wave digestion inductively coupled plasma emission spectrography (ICP method) is measured the method for metal platinum content in the catalyzer, and it is made up of the following step:
Step 1. takes by weighing the sample 0.05-0.2 gram (being accurate to 0.00001 gram) of oven dry in the micro-wave digestion jar; add the wetting sample of 1-2 milliliter secondary deionized water earlier; add 6-9 milliliter chloroazotic acid again, build lid, insert in the protective sleeve and put the safety spring sheet; compress whole counteracting tank; preparing blank sample simultaneously, put into microwave dissolver then and carry out Specimen eliminating, can not be sample blank liquid in the master control counteracting tank; the master control counteracting tank has temperature sensor and pressure transducer
Step 2. starts microwave dissolver, opens program control system and with program setting is: pressure 25-40bar, power 300-700W, heating schedule are to be warming up to 200-220 ℃, 25-40 minute constant temperature in 5-10 minute, cooling,
After step 3. was cleared up EOP (end of program), temperature shows then opened microwave dissolver when reaching 40 ℃ of left and right sides, and taking out counteracting tank and being placed on temperature is on 140 ℃ ± 10 ℃ the electric hot plate, acid solution to be rushed to about 2ml, 10ml constant volume then,
The last ICP that opens of step 4., treat that instrument igniting complete stability is good after, set up the analytical approach of this sample according to the condition of work of ICP.At first enter institute and join standard solution, utilize the function that examine provided in the ICP winlab software, do the background correction of tested element Pt and check the situation of emission spectrum, find the interference of element-free.Carry out the test of instrument blank, standard model, sample blank and testing sample then successively.Computing machine is with the test result of direct display element.
According to formula: C=(Ci-C0) * V/M
In the formula: the content of metallic element in the C---catalyzer, ug/g
The content of this element of Ci---in test solution, ug/ml
The content of this element of C0---in blank solution, ug/ml
The volume of V---test solution, ml
M---takes by weighing the quality of catalyst sample, g
Calculating can get the platinum content in the raw catalyst.
This method can shorten to 3-4 hour with the 1-1.5 days original sample preparation time (even longer); Only use the acid solution of 7-10 milliliter, saved cost of determination, reduced to the pollution of environment with to the injury of human body; The sample preparation step is simple, has alleviated labour intensity; Need not to add FeCl
3Solution has been avoided introducing more error, has improved the accuracy of measuring, and has certain economic benefits and social benefit.
Description of drawings
Fig. 1 is the ICP emission spectrum spectrogram of elements platinum;
Fig. 2 is a sample micro-wave digestion conditional curve, and wherein T is the temperature control curve in the digestion process; P is the pressure control curve in the digestion process; W is a variable power curve in the digestion process.
Embodiment
Further specify the present invention by the following examples.
Test used instrument and equipment:
The Optima3000 of inductive coupling plasma emission spectrograph U.S. PE company;
Microwave dissolver U.S. Milestone company;
Temperature range 0-250 ℃ in electric hot plate U.S. Labtech company;
The sub-1810-B of the company limited type of Jintan, quartzy automatic dual pure water distiller Jiangsu hundred million energisings;
The electronic balance Sartorius LE225D of company range of weighing 0.1mg-220g.
The experiment agents useful for same:
The secondary deionized water self-control;
Chloroazotic acid hydrochloric acid: nitric acid=3: 1 (volume ratio);
Platinum element standard solution 1000ppm State Standard Matter Research Centre.
The condition of work of ICP:
The optimal analytical line of Pt element is 265.945nm;
Emissive power: 1300W;
Height of observation: 15mm;
Plasma gas flow rate: 15L/min;
Secondary air amount: 0.4L/min;
Atomization gas flow: 0.7L/min
Peristaltic pump speed: 1.7ml/min
Metal platinum Determination on content in the useless agent of embodiment 1. catalytic reforming catalysts
This catalyst sample that takes by weighing the 0.1224g drying adds 1ml secondary deionized water and 8ml chloroazotic acid then successively in the micro-wave digestion jar, assemble counteracting tank, prepares blank sample simultaneously; Open microwave dissolver, with program setting be: pressure 30bar, power 500W, 200 ℃ of temperature, heating schedule are after being warming up to 200 ℃ in 10 minutes, constant temperature 30 minutes, cooling.Wait to clear up and finish, when temperature is reduced to room temperature, take out counteracting tank, on electric hot plate, steam, last 10ml constant volume to 2ml.Platinum content is 14.8ug/ml in the ICP test solution, and metal platinum content is 2875ug/g in the sample by calculating at last.
Only use 8 milliliters of chloroazotic acid in the sample preparation, add and catch up with the acid treatment time to need 3-4 hour, test procedure is simple.
The mensuration of platinum content in the oil plant at the bottom of 2. jars of the embodiment
Take by weighing the sample of 0.05434 gram after the drying in the micro-wave digestion jar, add 2 ml deionized water successively, 6 milliliters of chloroazotic acid assemble digestion system, prepare sample blank liquid simultaneously.Open the power supply of counteract appearance, be: pressure 25bar, power 300W, be warming up to 200 ℃, constant temperature in 5 minutes 30 minutes, cooling program setting.After clearing up end, on electric hot plate, steam to 2 milliliters last 10 milliliters of constant volumes.Platinum content 11.7ug/ml in the ICP test solution calculates that metal platinum content is 2153ug/g in the sample.
The mensuration of platinum content among residual Jiao of embodiment 3. platinum catalysts
Take by weighing the sample of 0.1007 gram after the drying in the micro-wave digestion jar, add 1 ml deionized water successively and 8 milliliters of chloroazotic acid assemble microwave digestion system, prepare sample blank liquid simultaneously.Open microwave dissolver, be: pressure 30bar, power 500W, be warming up to 200 ℃, constant temperature in 5 minutes 30 minutes, cooling program setting.Clear up the end back and on electric hot plate, steam to 2 milliliters 10 milliliters of constant volumes.The ICP test result is 19.3ug/ml, calculates that platinum content is 1913ug/g in this sample.
The test of tenors such as embodiment 4.EA-301A bottom head place thing platinum
Take by weighing the sample of 0.0963 gram after the drying in the micro-wave digestion jar, add 1 ml deionized water successively and 7 milliliters of chloroazotic acid assemble microwave digestion system, prepare sample blank liquid simultaneously.Open microwave dissolver, be: pressure 35bar, power 500W, be warming up to 210 ℃, constant temperature in 10 minutes 30 minutes, cooling program setting.Clear up the end back and on electric hot plate, steam to 1.5 milliliters 10 milliliters of constant volumes.The ICP test result is 20.1ug/ml, calculates that platinum content is 2091ug/g in this sample.
Sample preparation is simple, clears up fully, saves time, saves reagent.
Embodiment 5
The mensuration of metal platinum in the isomerization catalyst
Take by weighing the sample of 0.0641 gram after the drying in the micro-wave digestion jar, add 2 ml deionized water successively and 6 milliliters of chloroazotic acid assemble microwave digestion system.Open microwave dissolver, be: pressure 40bar, power 500W, be warming up to 220 ℃, constant temperature in 10 minutes 25 minutes, cooling program setting.Clear up the end back and on electric hot plate, steam to 2 milliliters 10 milliliters of constant volumes.The ICP test result is 20.5ug/ml, calculates that platinum content is 3198ug/g in this sample.
Embodiment 6
Platinum content is measured in the catalyzer of reformation North Area
Take by weighing the sample of 0.1592 gram after the drying in the micro-wave digestion jar, add 1 ml deionized water successively and 8 milliliters of chloroazotic acid assemble microwave digestion system.Open microwave dissolver, be: pressure 35bar, power 700W, be warming up to 200 ℃, constant temperature in 5 minutes 40 minutes, cooling program setting.Clear up the end back and on electric hot plate, steam to 2 milliliters 10 milliliters of constant volumes.The ICP test result is 37.9ug/ml, calculates that platinum content is 2382ug/g in this sample.
Embodiment 7
Metal platinum Determination on content in old dose of the reforming catalyst
Take by weighing the sample of 0.1962 gram after the drying in the micro-wave digestion jar, add 1 ml deionized water successively and 9 milliliters of chloroazotic acid assemble microwave digestion system.Open microwave dissolver, be: pressure 35bar, power 500W, be warming up to 210 ℃, constant temperature in 5 minutes 30 minutes, cooling program setting.Clear up the end back and on electric hot plate, steam to 2 milliliters 10 milliliters of constant volumes.The ICP test result is 55.5ug/ml, calculates that platinum content is 2830ug/g in this sample.
Embodiment 8
The assay of metal platinum in the new agent of reforming catalyst
Take by weighing the sample of 0.0904 gram after the drying in the micro-wave digestion jar, add 1 ml deionized water successively and 7 milliliters of chloroazotic acid assemble microwave digestion system.Open microwave dissolver, be: pressure 30bar, power 500W, be warming up to 200 ℃, constant temperature in 5 minutes 30 minutes, cooling program setting.Clear up the end back and on electric hot plate, steam to 2 milliliters 10 milliliters of constant volumes.The ICP test result is 27.6ug/ml, calculates that platinum content is 3048ug/g in this sample.
Above embodiment explanation: the sample preparation step is simple, solvent load is few, the processing time is short, has reduced experimentation cost, minimizing environmental pollution and to the injury of human body; ICP test element-free is disturbed, and need not to introduce medium, has avoided personal error, is a kind of quick, accurate analytical method.
Claims (1)
1. a micro-wave digestion inductively coupled plasma emission spectrography is measured the method for metal platinum content in the catalytic reforming catalyst, it is characterized in that it is made up of the following step:
The catalyst sample 0.05-0.2 that step 1. takes by weighing oven dry restrains in the micro-wave digestion jar; add the wetting catalyst sample of 1-2 milliliter secondary deionized water earlier; add 6-9 milliliter chloroazotic acid again; build lid; insert in the protective sleeve and put the safety spring sheet, compress whole counteracting tank, prepare blank sample simultaneously; put into microwave dissolver then and carry out Specimen eliminating
Step 2. starts microwave dissolver, opens program control system and with program setting is: pressure 25-40bar, power 300-700W, heating schedule are to be warming up to 200-220 ℃, 25-40 minute constant temperature in 5-10 minute, cooling,
After step 3. was cleared up EOP (end of program), temperature shows then opened microwave dissolver when reaching 40 ℃ of left and right sides, and taking out counteracting tank and being placed on temperature is on 140 ℃ ± 10 ℃ the electric hot plate, acid solution to be rushed to about 2ml, 10ml constant volume then,
The last ICP that opens of step 4., treat that instrument igniting complete stability is good after, set up the analytical approach of this catalyst sample according to the condition of work of ICP,
According to formula: C=(Ci-C0) * V/M
In the formula: the content of platinum element in the C---catalyzer, ug/g
The content of Ci---platinum element in test solution, ug/ml
The content of C0---platinum element in blank solution, ug/ml
The volume of V---test solution, ml
M---takes by weighing the quality of catalyst sample, g
Calculating can get the platinum content in the catalyst sample.
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| EP0447747A2 (en) * | 1990-02-27 | 1991-09-25 | Cytec Technology Corp. | Apparatus and method for injecting compounds in plasma for ICP-OES analysis |
| CN1128352A (en) * | 1992-11-22 | 1996-08-07 | 华南环境科学研究所 | COD determination method by means of microwave sealing digestion and dissolution and sealing tank |
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