CN116296661A - Preparation method of carbon-containing high-purity gold standard sample - Google Patents
Preparation method of carbon-containing high-purity gold standard sample Download PDFInfo
- Publication number
- CN116296661A CN116296661A CN202310115414.8A CN202310115414A CN116296661A CN 116296661 A CN116296661 A CN 116296661A CN 202310115414 A CN202310115414 A CN 202310115414A CN 116296661 A CN116296661 A CN 116296661A
- Authority
- CN
- China
- Prior art keywords
- carbon
- purity gold
- purity
- standard sample
- plating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 129
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000010931 gold Substances 0.000 claims abstract description 61
- 229910052737 gold Inorganic materials 0.000 claims abstract description 61
- 238000007747 plating Methods 0.000 claims abstract description 32
- 239000011159 matrix material Substances 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 22
- YQCIWBXEVYWRCW-UHFFFAOYSA-N methane;sulfane Chemical compound C.S YQCIWBXEVYWRCW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 7
- 239000004917 carbon fiber Substances 0.000 claims abstract description 7
- 238000012360 testing method Methods 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000011261 inert gas Substances 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 238000009835 boiling Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 239000002356 single layer Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000010309 melting process Methods 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 239000012466 permeate Substances 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 7
- 239000012535 impurity Substances 0.000 abstract description 4
- GUWKQWHKSFBVAC-UHFFFAOYSA-N [C].[Au] Chemical compound [C].[Au] GUWKQWHKSFBVAC-UHFFFAOYSA-N 0.000 abstract description 3
- 239000006184 cosolvent Substances 0.000 abstract description 3
- 239000010970 precious metal Substances 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 238000002207 thermal evaporation Methods 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000003908 quality control method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000011363 dried mixture Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
- G01N33/2022—Non-metallic constituents
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a preparation method of a carbon-containing high-purity gold standard sample, which comprises the steps of preparing a carbon-free high-purity gold matrix material; plating carbon on the surface of the high-purity gold matrix material by using high-purity carbon fibers in a vacuum carbon plating instrument; the carbon plating times are controlled, so that a series of high-purity gold standard samples with gradient carbon content can be obtained, the high-purity gold standard samples are used for calibrating a high-temperature tube furnace combustion-infrared carbon sulfur instrument, drawing a trace carbon standard working curve, and determining trace carbon in high-purity gold samples with unknown content. The invention realizes fixed value tracing by adopting a vacuum carbon plating technology and adopting a high-temperature tube furnace combustion-infrared carbon-sulfur method; the carbon-containing high-purity gold standard sample can be formulated simply, quickly and with low cost, the high-purity gold carbon-containing standard sample matched with the matrix can be obtained, the accuracy of carbon content in the high-purity gold is improved, cosolvent impurities are not required to be brought in the use process, and the precious metal percentage recovery can be realized.
Description
Technical Field
The invention relates to the technical field of standard sample development, in particular to a preparation method of a carbon-containing high-purity gold standard sample.
Background
Along with the development of technology, the high-purity gold material is increasingly widely applied to the field of high-precision technology such as aerospace, chips, integrated circuit boards and the like, and simultaneously, lower requirements on the impurity content of the high-purity gold, in particular to carbon element, are also provided. At present, no technology for detecting trace carbon of high-purity gold is mature, no relevant detection standard exists in the existing national standard GB/T25933-2010 high-purity gold, and no reference standard sample for matrix matching for detecting trace carbon in high-purity gold and no report on a preparation method thereof are available.
Disclosure of Invention
The invention aims to provide a carbon-containing high-purity gold standard sample with traceable magnitude, easy preparation and high reproducibility, which provides magnitude traceability and quality control guarantee for a detection technology of trace carbon in high-purity gold and fills the technical gap of preparing the trace carbon standard sample in the high-purity gold.
The technical problems solved by the invention can be realized by adopting the following technical scheme:
the preparation method of the carbon-containing high-purity gold standard sample comprises the following steps:
step one: preparing a high-purity gold matrix material without carbon; putting the high-purity gold matrix material into a beaker, adding (1+1) nitric acid solution to permeate the high-purity gold matrix material, putting the beaker on an electric hot plate, heating to boil, taking out the high-purity gold matrix material after boiling for at least 5 minutes, washing with distilled water, drying, and storing in inert gas or vacuum environment for later use;
step two: plating carbon; plating carbon on the surface of the high-purity gold matrix material in the first step by using high-purity carbon fibers in a vacuum carbon plating instrument, wherein the weight increment of the high-purity gold matrix material after carbon plating is the carbon content of the sample; obtaining a series of high-purity gold standard samples with gradient carbon content by controlling carbon plating times;
step three: the method is used for calibrating the high-temperature tube furnace combustion-infrared carbon-sulfur instrument, drawing a trace carbon standard working curve by using the high-purity gold standard sample with the serial gradient carbon content obtained in the step two, measuring trace carbon in the high-purity gold sample with unknown content, and verifying the reliability of the carbon-containing high-purity gold standard sample by the correlation coefficient of the working curve, the standard point return test, the repeated test and the other types of metal standard sample comparison equivalent test.
Preferably, the preparation of the high-purity gold matrix material without carbon in the first step is to remove carbon from over 99.999% of high-purity gold by high-temperature treatment at 1150 ℃.
Preferably, the 1150 ℃ high temperature treatment is to adopt a tubular infrared carbon-sulfur instrument, directly melt the carbon-sulfur instrument in a quartz tube furnace at 1150 ℃, introduce oxygen in the high temperature melting process, and repeatedly burn until the oscillometric signal of an infrared detector is zero.
Preferably, the high-purity gold matrix material in the first step is rolled and trimmed into regular square sheets with the size of 1mm thick and 72mm multiplied by 72mm after high-temperature carbon removal, and each sheet has the weight of 1+/-0.05 g and the accuracy of 0.0001mg.
Preferably, the carbon plating in the second step is performed by placing the high-purity gold matrix material in the first step in a sample stage of the vacuum carbon plating apparatus in a neat single-layer arrangement.
Preferably, the high-purity carbon fiber for carbon plating in the second step has a diameter of 0.8mm and a carbon content of 99%.
Preferably, the carbon plating in the second step adopts a continuous heating mode, the automatic rotating speed of the sample table is 20 revolutions per minute, the vacuum degree of the vacuum chamber is 2.0Pa, the detection current of the evaporation source is 1.0A, and the detection voltage is 0.5V.
Preferably, the serial high-purity gold standard samples with gradient carbon content obtained in the second step are respectively placed in weighing bottles, and inert gas is filled or vacuum-pumping is carried out for preservation.
The beneficial effects of the invention are as follows:
1. the invention realizes fixed value tracing by adopting a vacuum carbon plating technology and adopting a high-temperature tube furnace combustion-infrared carbon-sulfur method; the carbon-containing high-purity gold standard sample can be formulated simply, quickly and with low cost, the high-purity gold carbon-containing standard sample matched with the matrix can be obtained, the accuracy of carbon content in the high-purity gold is improved, cosolvent impurities are not required to be brought in the use process, and the precious metal percentage recovery can be realized;
2. the high-purity gold standard sample with different carbon contents and stable carbon layers is prepared by a quantitative carbon plating method, and the quantitative tracing and quality control guarantee is provided for the high-purity gold trace carbon detection technology; meanwhile, a trace carbon working curve is established by using high-temperature tube furnace combustion-infrared carbon-sulfur instrument equipment, the correlation coefficient is more than 0.999, the standard point return error is < +/-0.00003%, the carbon quantity in the steel standard sample is measured through the curve, and the test result is within the tolerance range of the carbon content in the steel standard sample.
Detailed Description
The present invention will be described in further detail with reference to examples, but embodiments of the present invention are not limited thereto.
The invention relates to a preparation method of a carbon-containing high-purity gold standard sample, which comprises the following steps:
step one: and (3) preparing a high-purity gold slice sample.
High-purity gold (99.999%) is subjected to high-temperature treatment at 1150 ℃ to remove carbon, the high-purity gold is directly melted at 1150 ℃ in a quartz tube furnace by a tube type infrared carbon-sulfur instrument, oxygen is introduced in the high-temperature melting process about 1min, and carbon dioxide generated by high-temperature combustion is fed into the infrared carbon-sulfur instrument by taking oxygen as carrier gas, and is repeatedly combusted for 2 times in general, so that infrared signals can be zeroed, and the carbon is not contained.
The high-purity gold matrix material subjected to high-temperature carbon removal is rolled and trimmed into regular square sheets with the size of 1mm thick and the two smooth sides of 72mm multiplied by 72mm, and each sheet weighs 1+/-0.05 g and is accurate to 0.0001mg (using a ten-thousand balance). Putting the gold flakes into a beaker, adding the (1+1) nitric acid solution to the gold flakes, heating the beaker on an electric plate to boil, boiling for at least 5 minutes, taking out the gold flakes, washing the gold flakes with distilled water, drying the gold flakes, and then preserving the gold flakes in a weighing bottle filled with inert gas for standby, or placing the weighing bottle in a vacuum bag for vacuum pumping and preserving for standby.
Step two: and (5) plating carbon on the sheet sample.
The cleaned and dried gold chips in the first step are placed in a sample stage of a vacuum thermal evaporation carbon plating instrument to be orderly arranged in a single layer, high-purity carbon fibers (with the diameter of 0.8mm and the carbon content of 99%) are installed on an excitation electrode, a continuous heating mode is adopted, the automatic rotating speed of the sample stage is set to be 20 revolutions per minute, meanwhile, the instrument is started under the conditions that the vacuum degree of a vacuum chamber is selected to be 2.0Pa, the detection current of an evaporation source is selected to be 1.0A, and the detection voltage is selected to be 0.5V, and the instrument automatically carries out thermal evaporation carbon plating. And (3) carrying out carbon plating for different times according to the number of different carbon evaporation sources, so that gold flakes contain different carbon amounts, obtaining gold flakes with serial gradient carbon amounts, respectively placing the gold flakes with different carbon amounts in weighing bottles and filling inert gas for preservation, or placing the weighing bottles in a vacuum bag for vacuumizing and preserving.
Step three: testing of carbon-containing high-purity gold standard samples.
The high-purity gold standard samples with the carbon content in the series gradient prepared in the second step are respectively sent into a high-temperature tube furnace combustion-infrared carbon sulfur instrument device to measure the infrared absorption value, a trace carbon working curve is established, and the reproducibility of the carbon content under different preservation times is verified under good preservation conditions; and verifying that errors of carbon increment and measured values and carbon values of other non-high-purity gold metal standards meet tolerance requirements.
Since carbon-containing high purity gold of about 1ppm or less is placed in air, it is liable to cause a change in carbon content, and thus the present invention has high demands on environmental conditions and precision of balances. The vacuum bag is filled with the inert gas or placed in the vacuum bag, and the vacuum bag is vacuumized, so that the change of the carbon content is avoided, and the weighing bottle cannot be used for weighing when the weighing bottle is used for weighing by a precision balance. The preparation steps can be completed in clean rooms with clean grades of thousands or more, and any possible carbonaceous tools and containers cannot directly contact the sample.
Embodiment one:
high purity gold (99.999%) was decarbonized by high temperature treatment at 1150 ℃ to make regular square sheets of about 1mm thickness, 72mm x 72mm smooth on both sides, each weighing about 1g, accurate to 0.0001mg (weighed using a ten-thousand balance). Putting the gold slice into a beaker, adding a (1+1) nitric acid solution into the beaker, heating and boiling the mixture on an electric hot plate for 5 minutes, washing the mixture with distilled water, drying the mixture, and storing the dried mixture in a weighing bottle filled with inert gas for later use.
The three gold sheets are placed in a sample stage of a thermal evaporation carbon plating instrument to be orderly arranged in a single layer, the instrument is started, high-purity carbon fibers (with the diameter of 0.8mm and the carbon content of 99%) are installed on an excitation electrode, a continuous heating mode is adopted, the automatic rotating speed of the sample stage is set to be 20 revolutions per minute, meanwhile, the instrument is started under the conditions that the vacuum degree of a vacuum chamber is selected to be 2.0Pa, the detection current of an evaporation source is selected to be 1.0A and the detection voltage is selected to be 0.5V, and the instrument automatically performs thermal evaporation carbon plating. The carbon plating time (times) of each gold sheet is controlled to enable the carbon content to be inconsistent, the gold sheets plated with carbon are immediately weighed by a ten-million balance, the weight increment of the three gold sheets is respectively 1.5 mug, 2.8 mug and 5.0 mug, the carbon content of the series of high-purity gold standard samples is respectively 0.000150%, 0.000280% and 0.000500%, the standard samples are sequentially sent into a high-temperature tube furnace combustion-infrared carbon-sulfur instrument to measure the infrared absorption value, a trace carbon working curve is established by taking the carbon content as an ordinate and the infrared absorption value as an abscissa, the correlation coefficient of the working curve is 0.9992, and the steel standard samples are independently measured for 2 times to carry out accuracy test. The results are shown in Table 1:
table 1 test values for example one
| Standard sample name | Measurement/% | Average/% | Standard value% |
| YSBC21080-2-2008 | 0.000957、0.000994 | 0.000976 | 0.0010 |
| YSBC 1108-98 | 0.001607、0.001590 | 0.001598 | 0.0016 |
The results in Table 1 show that the measured value of the steel standard sample is consistent with the standard value, namely the standard sample developed by the invention has good accuracy.
Embodiment two:
according to the preparation method of the invention, 1 g+/-0.0001 mg of the carbon-free high-purity gold sheet is accurately weighed, high-purity gold matrix samples with different carbon contents are obtained by controlling carbon plating time (times), the carbon increment is respectively 0.9ug and 2.3ug, the corresponding carbon contents are respectively 0.000090% and 0.000230%, the carbon contents of the two samples are measured by using a working curve established in the first embodiment, and the measurement results are shown in Table 2:
table 2 test values for example two
| Carbon increment | Theoretical carbon content | Determination of carbon content | Difference value |
| 0.9ug/g | 0.000090％ | 0.000070％ | -0.00002％ |
| 2.3ug/g | 0.000230％ | 0.000250％ | 0.00002％ |
The test results in Table 2 show that the difference between the measured value and the theoretical value is < + -0.00003%, and the trace carbon measurement requirement can be satisfied.
Embodiment III:
the stability test was performed on three standard gold plate samples (containing 0.000150%, 0.000280% and 0.000500% carbon) with different carbon contents 2 times after 1 day, 5 days and 10 days, and the results are shown in table 3:
table 3 test values for example three
| 1 day/% | 3 days/% | 7 days/% |
| 0.000153、0.000144 | 0.000146、0.000158 | 0.000149、0.000152 |
| 0.000283、0.000276 | 0.000279、0.000278 | 0.000271、0.000274 |
| 0.000501、0.000515 | 0.000498、0.000511 | 0.000506、0.000502 |
The results in the table three show that the results are unchanged after the sample is placed for a certain time, and the standard sample developed by the invention has good stability.
According to the embodiment, the carbon-containing high-purity gold standard sample can be formulated simply, quickly and at low cost, the high-purity gold carbon-containing standard sample matched with the matrix can be obtained, the accuracy of carbon content in the high-purity gold is improved, cosolvent impurities are not required to be brought in the use process, and the precious metal percentage recovery can be realized. Meanwhile, a trace carbon working curve is established by using the high-temperature tube furnace combustion-infrared carbon-sulfur instrument equipment by adopting the carbon-containing high-purity gold standard sample, the correlation coefficient is more than 0.999, the standard point return error is < +/-0.00003%, the carbon quantity in the steel standard sample is measured by the curve, and the test result is within the tolerance range of the carbon content in the steel standard sample.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the technical scope of the present invention, so any minor modifications, equivalent changes and modifications made to the above embodiments according to the technical spirit of the present invention still fall within the scope of the present invention.
Claims (8)
1. The preparation method of the carbon-containing high-purity gold standard sample is characterized by comprising the following steps of:
step one: preparing a high-purity gold matrix material without carbon; putting the high-purity gold matrix material into a beaker, adding (1+1) nitric acid solution to permeate the high-purity gold matrix material, putting the beaker on an electric hot plate, heating to boil, taking out the high-purity gold matrix material after boiling for at least 5 minutes, washing with distilled water, drying, and storing in inert gas or vacuum environment for later use;
step two: plating carbon; plating carbon on the surface of the high-purity gold matrix material in the first step by using high-purity carbon fibers in a vacuum carbon plating instrument, wherein the weight increment of the high-purity gold matrix material after carbon plating is the carbon content of the sample; obtaining a series of high-purity gold standard samples with gradient carbon content by controlling carbon plating times;
step three: the method is used for calibrating the high-temperature tube furnace combustion-infrared carbon-sulfur instrument, drawing a trace carbon standard working curve by using the high-purity gold standard sample with the serial gradient carbon content obtained in the step two, measuring trace carbon in the high-purity gold sample with unknown content, and verifying the reliability of the carbon-containing high-purity gold standard sample by the correlation coefficient of the working curve, the standard point return test, the repeated test and the other types of metal standard sample comparison equivalent test.
2. The method for preparing the carbon-containing high-purity gold standard sample according to claim 1, wherein the method comprises the following steps: the preparation of the high-purity gold matrix material without carbon in the first step is to remove carbon from over 99.999 percent of high-purity gold by high-temperature treatment at 1150 ℃.
3. The method for preparing the carbon-containing high-purity gold standard sample according to claim 2, wherein the method comprises the following steps: the 1150 ℃ high temperature treatment for removing carbon adopts a tubular infrared carbon-sulfur instrument, and is directly melted in a quartz tubular furnace at 1150 ℃, oxygen is introduced in the high temperature melting process, and the combustion is repeated until the oscillometric signal of an infrared detector is zero.
4. The method for preparing the carbon-containing high-purity gold standard sample according to claim 1, wherein the method comprises the following steps: the high-purity gold matrix material is rolled and trimmed into regular square sheets with the size of 1mm thick and 72mm multiplied by 72mm after high-temperature carbon removal, and the weight of each sheet is 1+/-0.05 g, and the accuracy is 0.0001mg.
5. The method for preparing a carbon-containing high-purity gold standard sample according to claim 4, wherein the method comprises the steps of: and step two, carbon plating, namely placing the high-purity gold matrix material in the step one into a sample stage of the vacuum carbon plating instrument for orderly single-layer arrangement.
6. The method for preparing the carbon-containing high-purity gold standard sample according to claim 1, wherein the method comprises the following steps: and step two, the high-purity carbon fiber for carbon plating has the diameter of 0.8mm and the carbon content of 99 percent.
7. The method for preparing a carbon-containing high-purity gold standard sample according to claim 6, wherein the method comprises the steps of: and step two, carbon plating adopts a continuous heating mode, the automatic rotating speed of a sample table is 20 revolutions per minute, the vacuum degree of a vacuum chamber is 2.0Pa, the detection current of an evaporation source is 1.0A, and the detection voltage is 0.5V.
8. The method for preparing the carbon-containing high-purity gold standard sample according to claim 1, wherein the method comprises the following steps: and (3) placing the high-purity gold standard samples with the carbon content in the series of gradients obtained in the step two in a weighing bottle respectively, and filling inert gas or vacuumizing for preservation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310115414.8A CN116296661A (en) | 2023-02-15 | 2023-02-15 | Preparation method of carbon-containing high-purity gold standard sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310115414.8A CN116296661A (en) | 2023-02-15 | 2023-02-15 | Preparation method of carbon-containing high-purity gold standard sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN116296661A true CN116296661A (en) | 2023-06-23 |
Family
ID=86814130
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310115414.8A Pending CN116296661A (en) | 2023-02-15 | 2023-02-15 | Preparation method of carbon-containing high-purity gold standard sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116296661A (en) |
-
2023
- 2023-02-15 CN CN202310115414.8A patent/CN116296661A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112697777A (en) | Method for determining content of lithium, sodium, magnesium and calcium in uranium compound | |
| CN112834487A (en) | Method for rapidly determining contents of chromium and iron in nickel-based superalloy by ICP-OES (inductively coupled plasma-optical emission spectrometry) | |
| CN116296661A (en) | Preparation method of carbon-containing high-purity gold standard sample | |
| Becker et al. | The silicon-28 path to the Avogadro constant-first experiments and outlook | |
| CN113984693B (en) | Method for measuring residual quantity of harmful heavy metal in printing ink | |
| CN114184445B (en) | Method for measuring content of residual metal element in OLED material | |
| CN114113463B (en) | Method for rapidly testing water content of sized and dried carbon fibers | |
| CN114608931A (en) | Pretreatment method for determining silver in soil and sediment by inductively coupled plasma mass spectrometry | |
| CN113138175A (en) | Method for determining carbon content in niobium-tungsten alloy | |
| CN113607536A (en) | Method for simultaneously detecting 13 elements in spectinomycin hydrochloride injection by ICP-MS (inductively coupled plasma-mass spectrometry) | |
| CN113406026A (en) | Method for measuring content of potassium oxide in fertilizer by using flame atomic absorption spectrometer | |
| CN108593696B (en) | Method for determining trifluoroacetic acid residue in polypeptide by using quantitative nuclear magnetism | |
| Gramlich et al. | Isotopic variations in commercial high-purity gallium | |
| Van Audenhove et al. | Deposition by electron bombardment and weighing under vacuum of thin high purity boron layers | |
| CN116858800A (en) | Analysis method for trace carbon and sulfur elements in high-purity metal | |
| CN110631874A (en) | Sample pretreatment method for determining content of silicon element in polymer and method for determining content of silicon element in polymer | |
| CN117388043B (en) | Method for dissolving single-particle sphene and (uranium-thorium)/helium annual method of single-particle sphene | |
| CN114814040B (en) | Method for detecting residual quantity of methyl bromide in tea | |
| CN113218816B (en) | Method for testing density of unknown gas at different temperatures by using thermogravimetric method | |
| CN1166944C (en) | Method for detecting content arsenic in water | |
| CN116773511A (en) | Method for detecting phosphorus content of industrial silicon powder | |
| CN112630178B (en) | Method for determining trace zinc and nickel in boric acid water sample by graphite furnace atomic absorption method | |
| RU2817517C1 (en) | Method of studying kinetics of interaction of hydrogen with sample of metal or alloy and installation for its implementation | |
| CN114460065A (en) | Method for measuring strontium in deoxidizer such as silicon-aluminum-calcium-barium, silicon-aluminum-barium, silicon-calcium-barium and the like | |
| Hodgkinson et al. | Contact and contactless electrical conductivity measurements on the liquid semiconductor systems In-Te and Sb-Tc |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |