CN107036858A - The sample preparation methods of material containing noble metal powder - Google Patents
The sample preparation methods of material containing noble metal powder Download PDFInfo
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- CN107036858A CN107036858A CN201611003184.2A CN201611003184A CN107036858A CN 107036858 A CN107036858 A CN 107036858A CN 201611003184 A CN201611003184 A CN 201611003184A CN 107036858 A CN107036858 A CN 107036858A
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- noble metal
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- metal powder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to noble metal secondary resource comprehensive reutilization field, more particularly to the sample preparation methods of material containing noble metal powder.The sample preparation methods of material containing noble metal powder, are carried out successively as follows:A, material mixing;B, curtailed sampling;C, sample drying and determination of moisture;D, sample grinding;E, three-dimensional blender device batch mixing;Eight points of F, sample.The present invention can guarantee that the low-volume samples obtained from sampling and small lot noble metal powder material carry out sample preparation, obtain less than 100 grams samples, it is ensured that final sample is representative and is adapted to analysis detection.
Description
Technical field
The present invention relates to noble metal secondary resource comprehensive reutilization field, more particularly to the sample of material containing noble metal powder
Preparation method.
Background technology
Noble metal refers mainly to gold, silver and platinum group metal(Ruthenium, rhodium, palladium, osmium, iridium, platinum)Deng 8 kinds of metallic elements.These metals
Most of color and lusters for possessing beauty, the resistance to chemicals is quite big, is difficult to cause chemical reaction under general condition.
Noble metal secondary resource enormous amount, source is complicated, and material properties, classification is different, and value is expensive, accurate evaluation
Its value is the basis of fair deal, is the core procedure of noble metal secondary resource comprehensive utilization.Noble metal secondary resource material
The core of appraisement system is that bullion content is determined, bullion content determines mainly there are 3 steps:(1)Sampling technique and equipment;
(2)Sample preparation technology and device;(3)Analysis and detection technology and equipment.Noble metal of the sampling equipment from single batch enormous amount
In secondary resource material, sample representative in tens of kilograms is obtained, the step is the core of noble metal secondary resource production
The heart, factory building point takes up an area greatly, and equipment investment is big, it is necessary to the design of science, automaticity height, low in the pollution of the environment, sample representativeness
High the advantages of, with high content of technology, sampling equipment research and development of the current China to noble metal secondary resource material are relatively weak, and the country does not have
Have and produce large-scale sampling equipment.Sample preparation technology and device are that the sample obtained from sampling equipment is homogenized, division
Process, the material of the examples representative Huge value in x-100 grams, therefore operating process are taken out from sample in tens of kilograms
It is long, operate especially fine.Analysis and detection technology and equipment, using science precision instrument, obtain thing by physics and chemical process
Expect the final step of noble metal Precise levels, the research starting of this respect China is early, and technology has been reached advanced world standards.Section
Learn, objective and just sampler and sample preparation technology can obtain representative sample, meet client's needs, obtain
It is the basis of Business survival and development to the competent of client.
For sampling the sample of obtained noble metal powder sample and small lot noble metal powder material in the past using random
Sampling method, quartering and pipe marksmanship etc., sampling method fall behind, it is difficult to obtain representative sample.
Chinese patent notification number:CN103398865A discloses a kind of taking for platinum group metal high-area carbon spent catalyst
Sample, method for making sample, realize the accuracy of platinum group metal high-area carbon spent catalyst samples' representativeness and sample preparation analysis.This
Invention comprises the following steps:(1)Splicing is weighed;(2)Once burn;(3)Secondary burning is weighed;(4)Ball milling mixing, homogenization;
(5)First sample curtailed sampling;(6)Ground and mixed;(7)Secondary sample in reduction device.The present invention finally gives and burnt by burning twice
Slag small volume, easily uniform, obtained sample is representative;Meanwhile, present invention sampling, the method stabilization of sample preparation, sampling speed
Degree is fast, sample amount is big, easy to operate, is easy to grasp, can obtain more truly reflecting the sample of overall material.
But it is only suitable for the carbon carrier sampling and sample preparation of field of fine chemical.Complicated to source, material properties, classification is different
Noble metal materials need more comprehensive method for making sample.
The content of the invention
It is an object of the invention to the deficiency for overcoming above-mentioned prior art, there is provided a kind of sample system of material containing noble metal powder
Preparation Method, can guarantee that the low-volume samples obtained from sampling and small lot noble metal powder material carry out sample preparation, is less than
100 grams of samples, it is ensured that final sample is representative and is adapted to analysis detection.This method is simple to operate, and sample representativeness is high, sample
Product weight is adapted to the requirement of analysis detection, and environment-friendly, the interests of enterprise and client can be guaranteed.
To achieve the above object, the technical solution adopted by the present invention is:
The sample preparation methods of material containing noble metal powder, are carried out successively as follows:
A, material mixing:5-20kg materials containing noble metal powder are carried out rotation mixing 10-30 minutes with 20-40 revs/min;
B, curtailed sampling:Division, sampling are carried out with three riffle samplers material mixed to step A, 10%-12% material enters 3
In individual sample bottle, remaining material is directly entered in splicing bucket;After the completion of division, sampling, 3 sample bottles, each sample are removed
Example weight is the material return precious metal smelting workshop in 150-800 grams, splicing bucket in bottle;
C, sample drying and determination of moisture:Appoint from 3 samples that step B has divided and take 2 samples weighings, then heat to 105
DEG C, 8-12 hours are incubated, then takes out to be cooled to after room temperature and weighs, the average value meter of example weight difference before and after 2 sample dryings
Calculate moisture;
D, sample grinding:It is any from step C to take a dried sample to be ground to diameter less than 100 μm;
E, three-dimensional blender device batch mixing:By sample ground step D batch mixing 10-20 minutes in three-dimensional blender device;
Eight points of F, sample:Carry out being divided into 8 samples, each sample again using eight riffle samplers sample mixed to step E
Weight is 10-100 grams.
Beneficial effects of the present invention:
1. the sample that the present invention finally gives is representative, sampling amount small volume.
2. the present invention can be directed to any noble metal powder material, detection accuracy is high, is that noble metal materials are fair, just hands over
Easily provide strong foundation.
3. inventive samples preparation method is stable, ripe, easy to operate, be easy to grasp.
4. the rotated mixing of material of the present invention and three-dimensional blender device batch mixing, can carry out fully mixing to material containing noble metal powder
Close, it is ensured that the reliability of sampling.
5. inventive samples are dried and determination of moisture, influence when moisture is symmetrically weighed in sample can be excluded, inspection is improved
Accuracy during survey.
Brief description of the drawings
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Embodiment 1
As shown in figure 1, the sample preparation methods of material containing noble metal powder, are carried out successively as follows:
The sample preparation methods of material containing noble metal powder, are carried out successively as follows:
A, material mixing:The mesh powder material of 5kg spent auto-catalysts 40 is put into mixing tank, the volume of mixing tank is 20
Rise, mixing tank is arranged on sample mixing machine, power-on, the rotating speed of sample mixing machine is 20 revs/min of progress rotation mixing, mixing time
For 10 minutes;
B, curtailed sampling:Division, sampling are carried out with three riffle samplers material mixed to step A, sampling bottle is screwed, and beat successively
Drive rotary switch, vibroswitch and carry out a point sample, vibrating feed after material conveying is finished in hopper and feeding groove, closes vibrations
And rotary switch, 10% material enters in 3 sample bottles, and remaining material is directly entered in splicing bucket;Division, sampling are completed
Afterwards, it is 150 grams to remove example weight in 3 sample bottles, each sample bottle, and the material in splicing bucket returns to precious metal smelting car
Between;
C, sample drying and determination of moisture:Appoint from 3 samples that step B has divided and take 2 samples weighings, be respectively put into 2 not
Become rusty in steel ware, weigh, be placed in drying box, then heat to 105 DEG C, be incubated 8 hours, then take out and be cooled to title after room temperature
The mean value calculation moisture of example weight difference before and after weight, 2 sample dryings;Influence when moisture is symmetrically weighed in sample is excluded, is carried
Accuracy during high detection;
D, sample grinding:It is any from step C take a dried sample to be ground in grinder, vibrated 100 μm of sieves
Net, the sample more than 100 μm continues to grind, until sample passes through screen cloth completely;
E, three-dimensional blender device batch mixing:Sample ground step D is loaded in sample mixing bottle, lid is covered and is put into three-dimensional blender device
, switch is opened, mixing time is 10 minutes, is closed after the completion of batch mixing, takes out mixing bottle;Material is sufficiently mixed, it is ensured that
The reliability of sampling;
Eight points of F, sample:Respectively sample is carried out using eight riffle samplers sample mixed to step E again, sampling is screwed
Bottle, and rotary switch, a vibroswitch progress point sample are opened successively, after material conveying is finished in hopper and feeding groove, close shake
8 sample bottles are removed after the completion of dynamic and rotary switch, all points of samples, sample is all divided equally in 8 sample bottles, each sample bottle
Interior example weight is 10 grams.
The sample finally given is representative, sampling amount small volume.Detection accuracy is high, be noble metal materials it is fair,
Arm's length transaction provides strong foundation.This method is stable, ripe, easy to operate, be easy to grasp.
Embodiment 2
The sample preparation methods of material containing noble metal powder, are carried out successively as follows:
A, material mixing:The mesh powder material of 12kg spent auto-catalysts 50 is put into mixing tank, the volume of mixing tank is
50 liters, mixing tank is arranged on sample mixing machine, power-on, and the rotating speed of sample mixing machine is 30 revs/min of progress rotation mixing, during batch mixing
Between be 20 minutes;
B, curtailed sampling:Division, sampling are carried out with three riffle samplers material mixed to step A, sampling bottle is screwed, and beat successively
Drive rotary switch, vibroswitch and carry out a point sample, vibrating feed after material conveying is finished in hopper and feeding groove, closes vibrations
And rotary switch, 11% material enters in 3 sample bottles, and remaining material is directly entered in splicing bucket;Division, sampling are completed
Afterwards, it is 450 grams to remove example weight in 3 sample bottles, each sample bottle, and the material in splicing bucket returns to precious metal smelting car
Between;
C, sample drying and determination of moisture:Appoint from 3 samples that step B has divided and take 2 samples weighings, be respectively put into 2 not
Become rusty in steel ware, weigh, be placed in drying box, then heat to 105 DEG C, be incubated 10 hours, then take out and be cooled to title after room temperature
The mean value calculation moisture of example weight difference before and after weight, 2 sample dryings;Influence when moisture is symmetrically weighed in sample is excluded, is carried
Accuracy during high detection;
D, sample grinding:It is any from step C take a dried sample to be ground in grinder, vibrated 100 μm of sieves
Net, the sample more than 100 μm continues to grind, until sample passes through screen cloth completely;
E, three-dimensional blender device batch mixing:Sample ground step D is loaded in sample mixing bottle, lid is covered and is put into three-dimensional blender device
, switch is opened, mixing time is 15 minutes, is closed after the completion of batch mixing, takes out mixing bottle;Material is sufficiently mixed, it is ensured that
The reliability of sampling;
Eight points of F, sample:Respectively sample is carried out using eight riffle samplers sample mixed to step E again, sampling is screwed
Bottle, and rotary switch, a vibroswitch progress point sample are opened successively, after material conveying is finished in hopper and feeding groove, close shake
8 sample bottles are removed after the completion of dynamic and rotary switch, all points of samples, sample is all divided equally in 8 sample bottles, each sample bottle
Interior example weight is 60 grams.
The sample finally given is representative, sampling amount small volume.Detection accuracy is high, be noble metal materials it is fair,
Arm's length transaction provides strong foundation.This method is stable, ripe, easy to operate, be easy to grasp.
Embodiment 3
The sample preparation methods of material containing noble metal powder, are carried out successively as follows:
A, material mixing:The mesh powder material of 20kg spent auto-catalysts 60 is put into mixing tank, the volume of mixing tank is
50 liters, mixing tank is arranged on sample mixing machine, power-on, and the rotating speed of sample mixing machine is 40 revs/min of progress rotation mixing, during batch mixing
Between be 30 minutes;
B, curtailed sampling:Division, sampling are carried out with three riffle samplers material mixed to step A, sampling bottle is screwed, and beat successively
Drive rotary switch, vibroswitch and carry out a point sample, vibrating feed after material conveying is finished in hopper and feeding groove, closes vibrations
And rotary switch, 12% material enters in 3 sample bottles, and remaining material is directly entered in splicing bucket;Division, sampling are completed
Afterwards, it is 800 grams to remove example weight in 3 sample bottles, each sample bottle, and the material in splicing bucket returns to precious metal smelting car
Between;
C, sample drying and determination of moisture:Appoint from 3 samples that step B has divided and take 2 samples weighings, be respectively put into 2 not
Become rusty in steel ware, weigh, be placed in drying box, then heat to 105 DEG C, be incubated 12 hours, then take out and be cooled to title after room temperature
The mean value calculation moisture of example weight difference before and after weight, 2 sample dryings;Influence when moisture is symmetrically weighed in sample is excluded, is carried
Accuracy during high detection;
D, sample grinding:It is any from step C take a dried sample to be ground in grinder, vibrated 100 μm of sieves
Net, the sample more than 100 μm continues to grind, until sample passes through screen cloth completely;
E, three-dimensional blender device batch mixing:Sample ground step D is loaded in sample mixing bottle, lid is covered and is put into three-dimensional blender device
, switch is opened, mixing time is 20 minutes, is closed after the completion of batch mixing, takes out mixing bottle;Material is sufficiently mixed, it is ensured that
The reliability of sampling;
Eight points of F, sample:Respectively sample is carried out using eight riffle samplers sample mixed to step E again, sampling is screwed
Bottle, and rotary switch, a vibroswitch progress point sample are opened successively, after material conveying is finished in hopper and feeding groove, close shake
8 sample bottles are removed after the completion of dynamic and rotary switch, all points of samples, sample is all divided equally in 8 sample bottles, each sample bottle
Interior example weight is 100 grams.
The sample finally given is representative, sampling amount small volume.Detection accuracy is high, be noble metal materials it is fair,
Arm's length transaction provides strong foundation.This method is stable, ripe, easy to operate, be easy to grasp.
Claims (1)
1. the sample preparation methods of material containing noble metal powder, it is characterised in that carry out successively as follows:
A, material mixing:5-20kg materials containing noble metal powder are carried out rotation mixing 10-30 minutes with 20-40 revs/min;
B, curtailed sampling:Division, sampling are carried out with three riffle samplers material mixed to step A, 10%-12% material enters 3
In individual sample bottle, remaining material is directly entered in splicing bucket;After the completion of division, sampling, 3 sample bottles, each sample are removed
Example weight is the material return precious metal smelting workshop in 150-800 grams, splicing bucket in bottle;
C, sample drying and determination of moisture:Appoint from 3 samples that step B has divided and take 2 samples weighings, then heat to 105
DEG C, 8-12 hours are incubated, then takes out to be cooled to after room temperature and weighs, the average value meter of example weight difference before and after 2 sample dryings
Calculate moisture;
D, sample grinding:It is any from step C to take a dried sample to be ground to diameter less than 100 μm;
E, three-dimensional blender device batch mixing:By sample ground step D batch mixing 10-20 minutes in three-dimensional blender device;
Eight points of F, sample:Carry out being divided into 8 samples, each sample again using eight riffle samplers sample mixed to step E
Weight is 10-100 grams.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111426800A (en) * | 2020-04-30 | 2020-07-17 | 鞍钢股份有限公司 | Method for evaluating uniformity of mixed materials |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103398865A (en) * | 2013-07-24 | 2013-11-20 | 贵研资源(易门)有限公司 | Sampling and sample preparation method of platinum group metal-containing carbon support dead catalyst |
-
2016
- 2016-11-15 CN CN201611003184.2A patent/CN107036858A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103398865A (en) * | 2013-07-24 | 2013-11-20 | 贵研资源(易门)有限公司 | Sampling and sample preparation method of platinum group metal-containing carbon support dead catalyst |
Non-Patent Citations (2)
Title |
---|
GEORGE J.ANTOS,ABDULLAH M.AITANI: "《石油催化重整》", 31 October 2009, 中国石化出版社 * |
杨宗坡,张鸿绪等: "二升三维运动高效混料器", 《粉末冶金技术》 * |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111426800A (en) * | 2020-04-30 | 2020-07-17 | 鞍钢股份有限公司 | Method for evaluating uniformity of mixed materials |
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Application publication date: 20170811 |