CN106092693B - A kind of preparation method of gold loaded carbon gold analytical standard substance - Google Patents
A kind of preparation method of gold loaded carbon gold analytical standard substance Download PDFInfo
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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
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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
- G01N1/38—Diluting, dispersing or mixing samples
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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
- G01N2001/2893—Preparing calibration standards
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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
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
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Abstract
The invention discloses a kind of preparation method of gold loaded carbon gold analytical standard substance, this method may include charcoal slurry preparation, gold absorption, washing filtering, drying, it is secondary mix and etc..Pass through the preparation method of gold loaded carbon gold analytical standard substance provided by the present application, gold loaded carbon gold analytical standard substance can be made, most effective quality monitoring means are provided for the test of gold loaded carbon sample analysis, and then preferably monitor gold extraction process process, it is horizontal to improve wet assay of gold measuring technology, the economic benefit for improving test industry, gold mine etc., improves resource utilization.With important social effect and economic significance.
Description
Technical field
The present invention relates to standard matter preparing technology fields, more particularly to a kind of system of gold loaded carbon gold analytical standard substance
Preparation Method.
Background technique
It extracts gold from both at home and abroad at present, carbon-in-pulp process is widely applied and dump leaching method, this extraction of gold process are required using activity
Charcoal extracts gold, if charcoal ADSORPTION OF GOLD amount is relatively low (mentioning charcoal in advance), will increase enterprise's production cost, if charcoal ADSORPTION OF GOLD amount is satiated
With golden loss will be caused, moreover, no longer ADSORPTION OF GOLD, charcoal residence time in ore pulp is too long, charcoal after absorption reaches equilibrium concentration
Abrasion are big, and gold loss is big.Therefore, in order to accurately control gold absorption, gold loaded carbon extraction, gold loaded carbon parsing technological parameter, money is improved
Source utilization rate, it is necessary to which the gold content for accurately knowing gold loaded carbon carries out analysis test to gold loaded carbon.The test of gold loaded carbon gold content is
It is no be validity test, can satisfy purposes, can test result be comparable, can obtain it is polygon adopt, recognize each other, these are all
Gold loaded carbon gold analysis method is carried out using gold loaded carbon gold analytical standard substance and is tested using gold loaded carbon gold standard material as foundation
Card, analysis quality monitoring, instrumental correction, are to guarantee high-quality measurement result, realize the weight of analysis Measurement reliability and validity
Want technical measures.Currently, it is very big to the analysis testing requirement amount of gold loaded carbon both at home and abroad, it is badly in need of gold loaded carbon gold analytical standard substance,
And it all there are no gold loaded carbon gold analytical standard substance both at home and abroad at present.
Summary of the invention
The present invention provides a kind of preparation methods of gold loaded carbon gold analytical standard substance.
The present invention provides following schemes:
A kind of preparation method of gold loaded carbon gold analytical standard substance, the method the following steps are included:
Step 1: charcoal slurry preparation, choosing has good applicability and representative active carbon, and the active carbon is carried out powder
Broken processing simultaneously crosses 200 meshes acquisition standard activity charcoal；During the standard activity charcoal is put into the adsorption tanks of agitating function；And to
In the adsorption tanks according to the quality of activated carbon than ratio the first wang aqueous solution of addition for 1:5, at normal temperature with 60 turns/
The speed divided, which stirs, obtains the charcoal slurry for 10~60 minutes；
Step 2: gold solution preparation, the proof gold for weighing certain mass are put into the first glass container, and it is molten that the second chloroazotic acid is added
First glass container is placed on electric hot plate and dissolves by heating the proof gold extremely dissolution the first gold solution of acquisition completely by liquid, then
First gold solution is divided into more parts of same volume with glass baler；More parts of first gold solutions are respectively put into multiple
In second glass container, and add water respectively into the multiple second glass container and stir evenly, it is molten to obtain more parts of the second gold medals
Liquid；
Step 3: gold absorption, the agitating function for starting the adsorption tanks are stirred, and make the charcoal slurry in mixing state；
More parts of second gold solutions are poured slowly into portionwise in the adsorption tanks, continues stirring and carries out the mixing of first time liquid, obtain
Uniform gold loaded carbon slurry；
Step 4: the gold loaded carbon slurry in the adsorption tanks is pumped supernatant liquor using sedimentation by washing filtering, to
Add water in the adsorption tanks and start agitating function, the gold loaded carbon is washed and starched to neutrality and stops adding water and stirring, continues to take out
Go supernatant liquor stopping when gold loaded carbon slurry is 1:2 with supernatant solid-to-liquid ratio；Start the agitating function in low speed shape
The gold loaded carbon is starched by being discarded in plastic containers in the adsorption tanks under state；Extraction is placed in the plastic containers again
Gold loaded carbon starch supernatant, stop when until gold loaded carbon slurry is in charcoal pureed, obtain charcoal pureed gold loaded carbon slurry；
Step 5: charcoal pureed gold loaded carbon slurry is placed in baking oven and dries by drying, obtains drying gold loaded carbon；
Step 6: mixing, and the drying gold loaded carbon is put into three-dimensional mixing machine and carries out second of solid-state and stirs and evenly mixs, both
Obtain the gold loaded carbon gold analytical standard substance.
Preferred: the content of chloroazotic acid is 1%~5% in first wang aqueous solution.
Preferred: the content of chloroazotic acid is 50% in second wang aqueous solution.
Preferred: the proof gold is the proof gold that mass fraction is more than or equal to 99.9%.
It is preferred: in the step 3, more parts of second gold solutions are poured slowly into portionwise in the adsorption tanks, are continued
Stirring carries out the mixing of first time liquid, obtains uniform gold loaded carbon slurry；Include:
Detect whether the gold loaded carbon slurry gold content reaches preset gold content value using atomic absorption spectrography (AAS), if it is
Then continue step 4, if not then repeat step 3 until acquisition the gold loaded carbon starch gold content value reach preset
Gold content value until carry out step 4 again.
It is preferred: in the step 5, charcoal pureed gold loaded carbon slurry to be placed in baking oven and is dried, obtained drying and carry
Golden charcoal；Include:
Charcoal pureed gold loaded carbon slurry is placed in baking oven and is dried under conditions of temperature is 155 DEG C.
It is preferred: in the step 6, the drying gold loaded carbon to be put into three-dimensional mixing machine and carries out second of solid-state and stirs
Mix mixing, both the gold loaded carbon gold analytical standard substance；Include:
The drying gold loaded carbon is put into three-dimensional mixing machine and carries out second of solid-state and stirs and evenly mixs, and carries out uniformity inspection
Survey, after detection is qualified both the gold loaded carbon gold analytical standard substance.
Preferred: the standard activity charcoal is high-quality cocoanut active charcoal.
Preferred: first glass container is identical as the volume of second glass container.
The specific embodiment provided according to the present invention, the invention discloses following technical effects:
By the invention it is possible to a kind of preparation method of gold loaded carbon gold analytical standard substance be realized, in a kind of implementation
Under, this method may include charcoal slurry preparation, gold solution preparation, gold absorption, washing filtering, drying, mix and etc..Pass through this Shen
The preparation method for the gold loaded carbon gold analytical standard substance that please be provided can make gold loaded carbon gold analytical standard substance, be gold loaded carbon
Sample analysis test provides most effective quality monitoring means, and then preferably monitors gold extraction process process, improves gold
Analysis and testing technology is horizontal, improves the economic benefit of test industry, gold mine etc., improves resource utilization.With important
Social effect and economic significance.
Certainly, it implements any of the products of the present invention and does not necessarily require achieving all the advantages described above at the same time.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment
Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field
Art personnel every other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment
A kind of preparation method of gold loaded carbon gold analytical standard substance provided in an embodiment of the present invention, this method includes following step
It is rapid:
Step 1: charcoal slurry preparation, choosing has good applicability and representative active carbon, and the active carbon is carried out powder
Broken processing simultaneously crosses 200 meshes acquisition standard activity charcoal；During the standard activity charcoal is put into the adsorption tanks of agitating function；And to
In the adsorption tanks according to the quality of activated carbon than ratio the first wang aqueous solution of addition for 1:5, at normal temperature with 60 turns/
The speed divided, which stirs, obtains the charcoal slurry for 10~60 minutes；The matrix of gold loaded carbon gold analytical standard substance provided by the present application is main
It is charcoal, the type and technical indicator of the common charcoal of gold is proposed according to all-mud cyanidation method, choosing has good applicability and representativeness, activity
Charcoal industry generally acknowledge, in extraction of gold process common high-quality cocoanut active charcoal (iodine sorption value >=950mg/g) be gold loaded carbon reference substance
Matter candidate.Crushing and processing are carried out to candidate and cross 200 mesh.And it goes to ensure that cocoanut active charcoal examination and test of products result reaches iodine absorption
Value 1012mg/g, 200 mesh of granularity, moisture 9.25%, ash content 6.7%.In practical applications, chloroazotic acid in first wang aqueous solution
Content be 1%~5%.
Step 2: gold solution preparation, the proof gold for weighing certain mass are put into the first glass container, and it is molten that the second chloroazotic acid is added
First glass container is placed on electric hot plate and dissolves by heating the proof gold extremely dissolution the first gold solution of acquisition completely by liquid, then
First gold solution is divided into more parts of same volume with glass baler；More parts of first gold solutions are respectively put into multiple
In second glass container, and add water respectively into the multiple second glass container and stir evenly, it is molten to obtain more parts of the second gold medals
Liquid；In practical applications, in order to accurately controlling the amount for preparing the gold solution, first glass container and described second
The volume of glass container is identical.In practical applications, the content of chloroazotic acid is 50% in second wang aqueous solution.The proof gold is
Mass fraction is more than or equal to 99.9% proof gold.For example, the proof gold that can accurately weigh certain mass is put into 3000ml glass burning
In cup, it is complete to dissolving that addition 1:1 chloroazotic acid dissolves by heating proof gold on electric hot plate, then takes the gold solution with 50ml glass baler point
50ml is placed in another 3000ml glass beaker, and tap water 3000ml is added, and stirs evenly that can both to obtain the second gold medal molten
Liquid.
Step 3: gold absorption, the agitating function for starting the adsorption tanks are stirred, and make the charcoal slurry in mixing state；
More parts of second gold solutions are poured slowly into portionwise in the adsorption tanks, continues stirring and carries out the mixing of first time liquid, obtain
Uniform gold loaded carbon slurry；Again when specific preparation, selects quality and content is the substance of standard, it can be ensured that the load produced
Golden charcoal slurry meets mark and requires.It is envisioned that the gold loaded carbon done may be caused due to various reasons during preparation
The case where desired value is not achieved in gold content in slurry, and in order to solve the problems, such as this, the embodiment of the present application can be provided using Atomic absorption
Whether the slurry gold content of gold loaded carbon described in spectroscopic methodology detection reaches preset gold content value, if it is continues step 4, such as
Fruit is not, repeat step 3 until the gold content value that the gold loaded carbon of acquisition is starched reaches preset gold content value again into
Row step 4.Specific detection method can be, and divides and takes the gold loaded carbon slurry 50ml, carry out doing rate, filtrate Atomic absorption point
Light photometer tests gold content, if gold content is 0ug/ml, illustrates that gold has been tightly held by activated carbon completely.It is carried out by this method
Check gold content value, it can be ensured that the gold content value of gold loaded carbon slurry reaches preset gold content value, provides standard for subsequent preparation
Substance can reduce the error that subsequent preparation occurs.
Step 4: the gold loaded carbon slurry in the adsorption tanks is pumped supernatant liquor using sedimentation by washing filtering, to
Add water in the adsorption tanks and start agitating function, the gold loaded carbon is washed and starched to neutrality and stops adding water and stirring, continues to take out
Go supernatant liquor stopping when gold loaded carbon slurry is 1:2 with supernatant solid-to-liquid ratio；Start the agitating function in low speed shape
The gold loaded carbon is starched by being discarded in plastic containers in the adsorption tanks under state；Extraction is placed in the plastic containers again
Gold loaded carbon starch supernatant, stop when until gold loaded carbon slurry is in charcoal pureed, obtain charcoal pureed gold loaded carbon slurry；
Step 5: charcoal pureed gold loaded carbon slurry is placed in baking oven and dries by drying, obtains drying gold loaded carbon；?
When specific implementation, charcoal pureed gold loaded carbon slurry is placed in baking oven and is dried under conditions of temperature is 155 DEG C.
Step 6: mixing, and the drying gold loaded carbon is put into three-dimensional mixing machine and carries out second of solid-state and stirs and evenly mixs, both
Obtain the gold loaded carbon gold analytical standard substance.In order to guarantee that the standard substance being made meets the requirements, the drying is carried
Golden charcoal, which is put into three-dimensional mixing machine, to carry out second of solid-state and stirs and evenly mixs, and carries out uniformity detection, after detection is qualified both institute
State gold loaded carbon gold analytical standard substance.The embodiment of the present application can provide two methods of the mixing of dry and wet, efficiently solve load gold
Charcoal is difficult to the technical problem mixed.It randomly selects increment (quality for being equivalent to minimum package) and carries out uniformity initial survey.Initial survey closes
After lattice, minimum package is distributed into using plastic bottle, 250g/ bottles, the shady and cool, place of drying is stored.It in practical applications, can be using this
Method design 5 gold loaded carbon standard specimens of preparation that application provides, each standard specimen 200kg need to use active carbon 250kg, according to active carbon
The volume of the property of heap density small (0.5g/cm3), 250kg activity powdered carbon is 0.5m3, and solid-to-liquid ratio 1:5 is made in 250kg active carbon
The charcoal slurry of (test obtains), then total weight is 1500kg, total volume 1.8m3.
Inspection for the gold loaded carbon gold analytical standard substance uniformity of method provided by the present application preparation:
Sampling mode selection, all preparation in quantitys and the standard substance for being distributed into minimum package unit, it is necessary to carry out uniformity
It examines.The number of unit extracted is examined there are enough representativenesses to population of samples.It is advised according to national standard reference material technology
The requirement of model JJG1006-94 extracts 25 units by the table of random numbers according to the unit number (800 < N < 900) of Bulk Samples,
Each unit takes 3 samples to carry out duplicate measurements in different parts, all data method of analysis of variance statistical checks to measuring
The uniformity of sample.
The selection of test method, the whether uniform used analysis method of selection check characteristic quantity gold undetermined is in addition to that will consider
Outside minimum sample mass size, the analysis method is also required to have not less than the precision of all valued methods and enough sensitive
Degree.How much minimum sample mass is by being used to that method used by uniformity is examined to determine.The gold loaded carbon point of existing known accuracy
There are two types of analysis methods, atomic absorption spectrography (AAS), Fire Assaying gravimetric method, considers the precision sensitivity of minimum sample mass and method,
Gold loaded carbon uniformity testing uses standard GB/T/T29509.1-2013 " gold loaded carbon chemical analysis method first in this project
Point: the measurement of gold amount " atomic absorption spectrography (AAS) in (2013-05-09 publication, 2014-02-01 implement), sample weighting amount is according to side
In method depending on minimum sample weighting amount as defined in different content section, butt method eliminates influence of the moisture to sample weighting amount.
Testing result assessment extracts 25 units, selection to carry out sample homogeneity assessment from gold loaded carbon overall cell
Atomic absorption spectrography (AAS) measures 25 groups of equally accurate test datas under the same conditions.Testing result such as table one:
One unit 10 of table-6
According to the requirement of " generic principles and Principle of Statistics of standard substance definite value " JJF1343-2012, using single factor test
Method of analysis of variance carries out uniformity assessment.
The sum of squares of deviations between unit
The sum of squares of deviations in unit
ν1=m-1
ν2=N-m
Variance S between unit1 2=Q1/ν1
Unit internal variance S2 2=Q2/ν2
Statistic F=S1 2/S2 2
In above formula, ν1=24, ν2=50, according to freedom degree and given significance, tables of critical values can be distributed by F and looked into
Obtain critical value F0.05 (24,50).5 gold loaded carbon standard specimens (ZJT-1, ZJT-2, ZJT-3, ZJT-4, ZJT-5) of this project development measure
F measured value < F0.05 (24,50), show that gold loaded carbon sample is uniform.
Gold loaded carbon uniformity assesses test data statistical result such as table two: unit 10-6
Table two
Inspection for the gold loaded carbon gold analytical standard substance stability of method provided by the present application preparation:
Stability is the essential attribute of standard substance, is the property that the characteristic value of standard substance changes over time, and is carrying gold
During charcoal Developments of certified reference samples, stability assessment can not only evaluate uncertainty of measurement relevant to gold loaded carbon stability,
And suitable storage and transport condition can be specified.
The a collection of sample of preparation simultaneously is stored under same environment, with the continuity of time, presses by stability monitoring method
According to " first close then dredge " principle respectively at 0,1,3,6 and 12 months, taken out at random from the sample for being distributed into minimum package unit
Sample is taken to be analyzed.Selection is not less than valued methods precision and the measurement method (GB/ with enough sensitivity
Atomic absorption spectrography (AAS) in T29509.1-2013 " gold loaded carbon chemical analysis method first part: the measurement of gold amount ") it carries out surely
Qualitative evaluation, and keep operation consistent with experiment condition.
STABILITY MONITORING result such as table three: unit 10-6
Table three
Standard substance has the function of saving, reappear and transmitting magnitude as a kind of measurement instrument.And the spy of standard substance
Whether property value is comparable in different times and spatially and reliability, the definite value measurement depending on this standard substance are
It is no to establish traceability.Definite value measurement is a pass during assert to the process and standard substance of standard substance assignment
Key link.Participating in definite value unit passed laboratory qualification certification, and definite value process is used through calibrating and in calibrating validity period
Interior equipment carries out analysis detection, ensure that the traceability of equipment；Standard solution used in definite value is certified reference material, is guaranteed
The traceability of standard solution；Definite value method therefor is theoretically upper with practice inspection proves that being accurately and reliably method
(national standard method GB/T29509.1-2013).
Selection to the standard substance definite value mode of method provided by the embodiments of the present application production:
The method of two kinds of verified accuracys of selection cooperates definite value by multiple laboratories.
Valued methods:
Using the Fire Assaying in GB/T29509.1-2013 " gold loaded carbon chemical analysis method first part: the measurement of gold amount "
Gravimetric method, flame atomic absorption spectrometry.
Cooperate definite value unit:
That participates in definite value has 9 units, is related to the multiple industry fields of geology, metallurgy, gold, with certain technology authority
Property, using two kinds of valued methods, 11 groups of value datas are obtained altogether.
1) Shandong Province's geological sciences research institute (Ministry of Land and Resources Jinan mineral resources supervisory detection center)
2) Experimental Inst of Geological Mineral Products, Shaanxi Prov. (Ministry of Land and Resources Xi'an mineral resources supervisory detection center)
3) Henan Rock Mineral Testing Centres (Ministry of Land and Resources Zhengzhou mineral resources supervisory detection center)
4) Heilongjiang Province's geological and mineral testing research institute (Ministry of Land and Resources Harbin mineral resources supervisory detection center)
5) Anhui Province's geological experiment research institute (Ministry of Land and Resources Hefei mineral resources supervisory detection center)
6) Central-South metallurgical geology research institute
7) Changchun Gold Research Institute's (national gold and silver and quality of item Supervision Test Center)
8) Jilin Prov. Academy of Metallurgy
9) Geology Scientific Institute, Jilin Province (Ministry of Land and Resources Changchun mineral resources supervisory detection center)
Measurement method description:
Fire Assaying gravimetric method: sample passes through calcination process, with Fire Assaying reagent through ingredient, melting, obtains appropriate quality
Lead button containing noble metal.Being blown by ash, which makes gold and silver close grain, deducts points with lead from obtained gold and silver closes grain after pernitric acid parting, uses
The content of gravimetric detemination gold.
Flame atomic absorption spectrometry: sample is after calcination is ashed, with aqua regia dissolution residue.In fire in diluted hydrochloric acid medium
At flame Atomic Absorption Spectrometer wavelength 242.8nm, using air-acetylene flame, the absorbance of gold is measured, based on calibration curve method
Calculate content.
Measurement process description:
Instrument: GGX-610 atomic absorption spectrophotometer, golden hollow cathode lamp.
Measuring condition: negative high voltage 335V；Lamp current 5mA；Air mass flow 5L/min；Acetylene flow 1L/min；Operation wavelength
242.8nm。
Goldstandard solution: weighing 1.0000g proof gold (mass fraction >=99.99%) in 100mL beaker, and 10mL king is added
Water (1+1), ground temperature are heated to being completely dissolved, remove and be cooled to room temperature.It moves into 1000mL volumetric flask, is diluted with water to scale,
It mixes.This goldstandard stock solution 1mL is containing 1mg gold.50.00mL goldstandard stock solution is pipetted in 500mL volumetric flask, is added
50mL hydrochloric acid (1+1), is diluted with water scale, mixes.This goldstandard solution 1mL is containing 100ug gold.
Analytical procedure: sample is placed in 100 DEG C~105 DEG C drying 1h, and is placed in drier and is cooled to room temperature.It weighs
Sample 0.5000g~1.0000g (as w (Au) < 1600g/t, weighs 1.0g sample；As w (Au) > 1600g/t, weigh
0.5g sample) in dry porcelain crucible, it moves into Muffle furnace.650 DEG C, slightly blow-on door are slowly risen by low temperature, under aerobic conditions
In 650 DEG C of calcination 1h~2h, until ashing completely, takes out crucible to room temperature.With residue in a small amount of water wetting crucible, 10mL is added
Chloroazotic acid (1+1) is steamed to close in water-bath, is removed slightly cold.It is added 10mL hydrochloric acid (1+1), heating dissolves salt, removes and is cooled to
Room temperature.Solution transfer is entered into constant volume in volumetric flask, is mixed.At Atomic Absorption Spectrometer wavelength 242.8, using air second flame, with
The zeroing of " zero " strength solution, measures test solution and the absorbance in company with sample blank, and the dense of corresponding gold is found from working curve
Degree.
Working curve is drawn: 0.00mL, 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL goldstandard solution are pipetted,
It is respectively placed in 100mL volumetric flask, is added 10mL hydrochloric acid (1+1), is diluted with water to scale, mix.Identical as sample solution
Under determination condition, with the zeroing of " zero " strength solution, the absorbance of series standard solution is measured.Using the concentration of gold as abscissa, inhale
Luminosity is that ordinate draws working curve.
Analyze the calculating of result: golden mass fraction w (Au) according to the following formula, numerical value is with 10-6It indicates:
In formula:
ρ --- golden concentration in test solution, unit are micrograms per millilitre (ug/mL)；
V----- test solution volume, unit are milliliter (mL)；
The quality of m----- sample, unit are gram (g).
The method (Fire Assaying gravimetric method, flame atomic absorption spectrometry) of two kinds of verified accuracys of selection, by 9 realities
Room cooperation definite value is tested, 11 groups of data are shared.
Cooperate definite value result such as table four: unit 10-6
Table four
When carrying out the statistical disposition and statistical check of data to value data, it is often based on the data and obeys normal state point
Cloth, therefore normal distribution inspection should be carried out to original independent determination data first during carrying out definite value and uncertainty evaluation
It tests.This project develops 5 gold loaded carbon standard substances altogether, and 9 laboratories provide 11 groups of data 44 solely to each standard substance
Vertical measurement result.Normal distribution-test is carried out to this data by summer Pyrrho-welker's method.
Lower target K value in formula is 1~n/2 when to wait pendulous frequencies n be even number；Then be 1 when pendulous frequency is odd number~
(n-1)/2；Coefficient a is specific quantity related with n and K.Inspection result such as table five:
Table five
| Location parameter | ZJT-1 | ZJT-2 | ZJT-3 | ZJT-4 | ZJT-5 |
| W | 0.97412 | 0.94954 | 0.9697 | 0.96953 | 0.9618 |
| W0.95(n,p) | 0.944 | 0.944 | 0.944 | 0.944 | 0.944 |
| W0.99(n,p) | 0.924 | 0.924 | 0.924 | 0.924 | 0.924 |
| Test parameter | ZJT-1 | ZJT-2 | ZJT-3 | ZJT-4 | ZJT-5 |
| W | 0.94334 | 0.93387 | 0.94686 | 0.95713 | 0.95728 |
| W0.95(n,p) | 0.85 | 0.85 | 0.85 | 0.85 | 0.85 |
| W0.99(n,p) | 0.792 | 0.792 | 0.792 | 0.792 | 0.792 |
The criterion of statistic W is, as W > W (n, p), then receiving the determination data is normal distribution.W (n, p) be with
Pendulous frequency n and the related numerical value of fiducial probability p.Above-mentioned inspection result shows 5 gold loaded carbon standard substance value data units
Interior and average data meets W > W (11,0.95), shows setting examination data fit normal distribution.
Comparison and verifying to the standard substance of method provided by the embodiments of the present application production
Send the gold loaded carbon standard substance (ZJT-1, ZJT-2, ZJT-3, ZJT-4, ZJT-5) randomly selected to Hebei province Di Kuang
It is examined outside one innings of central laboratory, Chinese metallurgical geology general bureau test center, to compare and verify.
Outer detection test result such as table six: unit 10-6
Table six
Determination to the standard substance asserting value of method provided by the embodiments of the present application production
The determination of standard substance asserting value (standard value) is using GB/T29509.1-2013 " gold loaded carbon chemical analysis method
First part: the measurement of gold amount " in Fire Assaying gravimetric method, flame atomic absorption spectrometry it is fixed by the cooperation of multiple laboratories
Value, value data carry out data processing according to JJF1343-2012 " generic principles and Principle of Statistics of standard substance definite value ",
Meeting each cell mean of normal distribution in value data is in the case that equally accurate is examined, each cell mean to be calculated, by average value
Average value is calculated again, finds out overall average, as standard value.
Overall average calculated result such as seven unit 10 of table-6
Table seven
| Test parameter | ZJT-1 | ZJT-2 | ZJT-3 | ZJT-4 | ZJT-5 |
| Average value (X) | 60.8 | 228.0 | 507.6 | 1528 | 3343 |
Expanded uncertainty calculated result such as eight unit 10 of table-6
Table eight
| Test parameter | ZJT-1 | ZJT-2 | ZJT-3 | ZJT-4 | ZJT-5 |
| UCRM (k=2) | 1.4 | 4.5 | 6.1 | 15 | 20 |
Complete definite value result should include two parts, the asserting value of standard substance and the expanded uncertainty of asserting value.I.e.
It indicates are as follows:
Y±UCRM
In formula:
Y------- standard value；
UCRM--- ----expanded uncertainty.
Standard substance definite value result such as table nine (taking k=2, corresponding fiducial probability 95%) unit 10-6
Table nine
| Test parameter | ZJT-1 | ZJT-2 | ZJT-3 | ZJT-4 | ZJT-5 |
| Standard value (Y) | 60.8±1.4 | 228.0±4.5 | 507.6±6.1 | 1528±15 | 3343±20 |
In short, gold loaded carbon gold can be made by the preparation method of gold loaded carbon gold analytical standard substance provided by the present application
Analytical standard substance, using it is natural and it is artificial synthesized combine technique, by two kinds of substances of active carbon and proof gold be made gold loaded carbon gold
Analytical standard material sample.Two kinds of hybrid techniques are mixed using liquid mixing and solid-state and carry out sample mixing, it is uniform to improve sample
Property.Using the storage of nearly dry state, dry state valued methods, avoid storage, transport, in use process gold loaded carbon rapidly, it is strong, a large amount of
It absorbs water and causes gold loaded carbon value unstable and problem of dispersing.Most effective quality monitoring hand is provided for the test of gold loaded carbon sample analysis
Section, and then gold extraction process process is preferably monitored, wet assay of gold measuring technology level is improved, test industry, gold are improved
The economic benefit in mine etc. improves resource utilization.With important social effect and economic significance.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention
It is interior.
Claims (7)
1. a kind of preparation method of gold loaded carbon gold analytical standard substance, which is characterized in that the described method comprises the following steps:
Step 1: charcoal slurry preparation, choosing has good applicability and representative active carbon, and the active carbon is carried out at crushing
It manages and crosses 200 meshes and obtain standard activity charcoal；The standard activity charcoal is high-quality cocoanut active charcoal；The high-quality cocoanut active charcoal
Examination and test of products result reaches iodine sorption value 1012mg/g, 200 mesh of granularity, moisture 9.25%, ash content 6.7%；The standard is living
Property charcoal is put into the adsorption tanks with agitating function；And into the adsorption tanks according to the quality of activated carbon than for 1:5's
The first wang aqueous solution is added in ratio, is stirred with 60 revs/min of speed obtain within 10~60 minutes the charcoal slurry at normal temperature；Described
The content of chloroazotic acid is 1%~5% in one wang aqueous solution；
Step 2: gold solution preparation, the proof gold for weighing certain mass are put into the first glass container, and the second wang aqueous solution is added,
First glass container is placed on electric hot plate and dissolves by heating the proof gold extremely dissolution the first gold solution of acquisition completely, then uses glass
First gold solution is divided into more parts of same volume by glass baler；More parts of first gold solutions are respectively put into multiple second
In glass container, and add water respectively into the multiple second glass container and stir evenly, obtains more parts of the second gold solutions；
Step 3: gold absorption, the agitating function for starting the adsorption tanks are stirred, and make the charcoal slurry in mixing state；By institute
It states more parts of the second gold solutions to be poured slowly into portionwise in the adsorption tanks, continues stirring and carry out the mixing of first time liquid, obtain uniform
Gold loaded carbon slurry；
Step 4: the gold loaded carbon slurry in the adsorption tanks is pumped supernatant liquor using sedimentation by washing filtering, to described
Add water in adsorption tanks and start agitating function, the gold loaded carbon is washed and starched to neutrality and stops adding water and stirring, continues to pump
Stopping when gold loaded carbon slurry is 1:2 with supernatant solid-to-liquid ratio of layer clear liquid；Start the agitating function under lower-speed state
The gold loaded carbon is starched by being discarded in plastic containers in the adsorption tanks；Extract the load being placed in the plastic containers out again
Golden charcoal starches supernatant, stops when until gold loaded carbon slurry is in charcoal pureed, obtains charcoal pureed gold loaded carbon slurry；
Step 5: charcoal pureed gold loaded carbon slurry is placed in baking oven and dries by drying, obtains drying gold loaded carbon；
Step 6: mixing, and the drying gold loaded carbon is put into three-dimensional mixing machine and carries out second of solid-state and stirs and evenly mixs, and both obtains institute
State gold loaded carbon gold analytical standard substance.
2. the method according to claim 1, wherein the content of chloroazotic acid is 50% in second wang aqueous solution.
3. the method according to claim 1, wherein the proof gold is that mass fraction is pure more than or equal to 99.9%
Gold.
4. the method according to claim 1, wherein in the step 3, by more parts of second gold solutions by
Part is poured slowly into the adsorption tanks, continues stirring and carries out the mixing of first time liquid, obtains uniform gold loaded carbon slurry；Include:
Detect whether gold loaded carbon slurry gold content reaches preset gold content value using atomic absorption spectrography (AAS), if it is after
It is continuous to carry out step 4, if not then repeating step 3 until the gold content value that the gold loaded carbon of acquisition is starched reaches preset gold
Step 4 is carried out until content value again.
5. the method according to claim 1, wherein charcoal pureed gold loaded carbon slurry is set in the step 5
It is dried in baking oven, obtains drying gold loaded carbon；Include:
Charcoal pureed gold loaded carbon slurry is placed in baking oven and is dried under conditions of temperature is 155 DEG C.
6. the method according to claim 1, wherein the drying gold loaded carbon is put into three in the step 6
Carry out second of solid-state in dimension mixing machine and stir and evenly mix, both the gold loaded carbon gold analytical standard substance；Include:
The drying gold loaded carbon is put into three-dimensional mixing machine and carries out second of solid-state and stirs and evenly mixs, and carries out uniformity detection,
After detection is qualified both the gold loaded carbon gold analytical standard substance.
7. the method according to claim 1, wherein first glass container and second glass container
Volume is identical.
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| CN102252935A (en) * | 2011-04-07 | 2011-11-23 | 广西地博矿业集团股份有限公司 | Chemical gravimetric method for determining content of gold in gold-loaded carbon |
| CN102549177A (en) * | 2009-07-01 | 2012-07-04 | 贵金属回收私人有限公司 | Smelting method |
| CN104034562A (en) * | 2014-05-05 | 2014-09-10 | 福建紫金矿冶测试技术有限公司 | Gold loaded carbon chemical component standard substance and preparation method thereof |
| CN104931575A (en) * | 2015-06-23 | 2015-09-23 | 河南省岩石矿物测试中心 | Analysis method for identifying gold, platinum and palladium in chemical sample |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102549177A (en) * | 2009-07-01 | 2012-07-04 | 贵金属回收私人有限公司 | Smelting method |
| CN102252935A (en) * | 2011-04-07 | 2011-11-23 | 广西地博矿业集团股份有限公司 | Chemical gravimetric method for determining content of gold in gold-loaded carbon |
| CN104034562A (en) * | 2014-05-05 | 2014-09-10 | 福建紫金矿冶测试技术有限公司 | Gold loaded carbon chemical component standard substance and preparation method thereof |
| CN104931575A (en) * | 2015-06-23 | 2015-09-23 | 河南省岩石矿物测试中心 | Analysis method for identifying gold, platinum and palladium in chemical sample |
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