CN117288886A - Method for measuring moisture content in titanium sponge - Google Patents
Method for measuring moisture content in titanium sponge Download PDFInfo
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- CN117288886A CN117288886A CN202311250216.9A CN202311250216A CN117288886A CN 117288886 A CN117288886 A CN 117288886A CN 202311250216 A CN202311250216 A CN 202311250216A CN 117288886 A CN117288886 A CN 117288886A
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- Prior art keywords
- sample
- titanium sponge
- moisture content
- samples
- titanium
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002245 particle Substances 0.000 claims abstract description 16
- 239000000284 extract Substances 0.000 claims abstract description 11
- 238000005259 measurement Methods 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 6
- 239000000523 sample Substances 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 238000004448 titration Methods 0.000 claims description 13
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 239000012488 sample solution Substances 0.000 claims description 2
- 125000000532 dioxanyl group Chemical group 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 abstract description 15
- 239000010936 titanium Substances 0.000 abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 10
- 230000001737 promoting effect Effects 0.000 abstract description 4
- 238000004364 calculation method Methods 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000005070 sampling Methods 0.000 abstract description 2
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 7
- 238000012360 testing method Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 241001411320 Eriogonum inflatum Species 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
- G01N31/168—Determining water content by using Karl Fischer reagent
-
- 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
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a method for measuring the moisture content in titanium sponge. The method comprises the steps of sample preparation, extract preparation, fischer-Tropsch method measurement and calculation, wherein sponge titanium samples are grouped according to different particle sizes, the sponge titanium samples are respectively measured, and then the water content of the samples is calculated through weighted average, so that inaccuracy of a result caused by sampling deviation is avoided. The invention can be used for guiding and improving the production process of the titanium sponge, improving the quality of titanium sponge products and promoting the upgrading of titanium industry products.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a method for measuring the moisture content in titanium sponge.
Background
The quality of the titanium sponge can be influenced by the moisture in the gaps on the surface of the titanium sponge, and the quality of the titanium sponge can be ensured by strictly testing the quality of the moisture in the titanium sponge. The moisture in the titanium sponge is removed, and the moisture content needs to be rapidly and accurately analyzed. Therefore, the analysis and control of the moisture in the titanium sponge are also key to the quality control of the titanium material. If the technical problem of analysis of the moisture content in the titanium sponge can be developed, the method is used for guiding and improving the production process, improving the quality of titanium sponge products, and has great economic benefit for promoting the upgrading of the titanium industry products, promoting the export of the titanium products and increasing the domestic and foreign market share of the titanium products.
In a moist air environment, the sponge titanium is easy to absorb moisture in the air, the moisture content absorbed by the sponge titanium is relatively low, the conventional oven method is quite complicated in measurement, inaccurate in measurement and long in time consumption, and the moisture in the sponge titanium is not completely analyzed and tested, so that the analysis requirement of the moisture in the sponge titanium can not be met.
Disclosure of Invention
The invention aims to provide a method for measuring the moisture in the titanium sponge, which can rapidly and accurately measure the moisture content in the titanium sponge, and the data obtained by the method can be used for analyzing and controlling the quality of products.
The invention is realized in the following way:
the method for measuring the moisture content in the titanium sponge comprises the following steps:
s1, sample preparation: preparing a sample with the particle size ranging from 0.1cm to 6cm from titanium sponge, and grouping the sample according to different particle sizes by using a classifying screen;
s2, preparation of an extract: weighing 1g-20g from a group of samples, placing the samples into a wide-mouth bottle, weighing until the sample is 0.0002 and g, covering the wide-mouth bottle with a rubber stopper, injecting 50.0-100.0 mL of organic extractant into the wide-mouth bottle by using a syringe, placing the wide-mouth bottle in an ultrasonic cleaner for cleaning for 30 min, standing for 15min, shaking or oscillating until the sample solution is uniform, taking part of the solution after the sample is slightly settled, placing the solution into a centrifuge tube with the rubber stopper for centrifugation, and taking the centrifugate as an extract for standby;
s3, determination: calculating the moisture content in the group of sample extracts by Fischer titration measurement;
s4, repeating the steps S1-S3 to obtain the moisture content of each group of samples, taking the weights of the samples of different groups as weights, and calculating a weighted average value to obtain the moisture content of the titanium sponge product.
Preferably, in the step S1, the titanium sponge is prepared into samples with the particle size ranging from 0.1cm to 3cm, and the samples are divided into six groups according to the particle size of 0.10 to 0.50cm,0.51 to 1.00cm,1.10 to 1.50cm,1.51 to 2.00cm,2.01 to 2.50cm and 2.51 to 3.0 cm by using a classifying screen;
preferably, the organic extractant in step S2 is any one of dioxane, absolute ethanol and methanol.
Preferably, step S2 is to weigh 1g from a set of samples, place into a 500mL jar, and inject 200.0. 200.0mL of the organic extractant as dioxane with a syringe.
Preferably, the detection limit of the measuring method is 10mg/kg.
According to the invention, the sponge titanium samples are grouped according to different particle sizes, the water content in the sponge titanium product is calculated through weighted average, inaccuracy of the test result caused by sampling deviation is avoided, and the water content in the extracted sample is calculated through titration measurement by adopting a Fischer-Tropsch method, so that the method is more accurate and more convenient than an oven method. The invention can be used for guiding and improving the production process of the titanium sponge, improving the quality of titanium sponge products and promoting the upgrading of titanium industry products.
Examples
The invention is further described in connection with the following detailed description. The following examples are given solely for the purpose of illustration and not as a definition of the limits of the invention, and it will be appreciated by those skilled in the art that modifications and equivalent substitutions of the invention are intended to be encompassed within the scope of the appended claims.
1. Preparing a titanium sponge sample: preparing titanium sponge into samples with the particle size ranging from 0.1cm to 3cm, and classifying the samples into samples with the particle size ranging from 0.10 cm to 0.50cm,0.51 cm to 1.00cm,1.10 cm to 1.50cm,1.51 cm to 2.00cm,2.01 cm to 2.50cm and 2.51 cm to 3.0 cm by using a classifying screen.
2. Preparing a titanium sponge sample extract: accurately weighing 1g of sample, placing into 500mL wide-mouth bottle with rubber stopper, weighing to 0.0002 g, covering with bottle stopper, injecting 50.0 mL dioxane with syringe, optionally replacing with absolute ethanol or methanol, placing into ultrasonic cleaner, ultrasonic treating for 30 min, standing for 15min, shaking or oscillating for several min, centrifuging part of the solution in centrifuge tube with rubber stopper after the sample is slightly settled, and collecting the centrifugate as extract.
3. And (3) measuring: discharging residual liquid in the titration container through the drain nozzle, adding 50mL of methanol into the titration container, wherein the dosage of the methanol is enough to submerge the electrode, switching on the power supply, switching on the electromagnetic stirrer, and titrating with the Karl Fischer reagent until the ammeter generates the same reading as the calibration, and keeping stable
1 min。
Taking out 5.0 mL dioxane extract from the centrifuge tube by using a syringe, injecting the extract into a titration container through a feeding hole of Karl Fei Xiuyi, titrating with Karl Fischer reagent to an end point, and recording the volume of the Karl Fischer reagent consumedV 1 ）。
When dioxane is used as the extractant, the residual liquid in the titration vessel should be discharged after three titrations, methanol is added, and the titration is carried out to the same end point by using Karl Fischer reagent. The next measurement is then performed.
In the same way, the volume of the Karl Fischer reagent consumed by 5.0. 5.0 mL dioxane was measuredV 2 ）。
c. Calculation of measurement results
Moisture contentωExpressed as mass fraction (%), calculated as formula (1):
wherein:
V 1 titration of the value of the volume of karl fischer reagent consumed by the 5.0 mL dioxane extraction solution in milliliters (mL);
V 2 titration of 5.0. 5.0 mL dioxaneThe volume of the Fischer reagent consumed is measured in milliliters (mL);
Tthe value of the titer of the Fischer reagent against water in milligrams per milliliter (mg/mL); different karl fischer reagents have less identical T values, which were calculated after titration using a syringe with 10 microliters of water added to the titration vessel.
T=m/V. Wherein: m-represents the mass of water added in milligrams (mg) and V-represents the volume of karl fischer reagent consumed in milliliters (mL) when calibrated.
mThe mass of the test specimen in grams (g).
4. Repeating the steps 1-3 to obtain the moisture content of each group of samples, taking the weights of the samples of different groups as weights, and calculating a weighted average value to obtain the moisture content of the titanium sponge product. The result of the calculation represents a 3-significant digit.
The measurement results of the moisture in the titanium sponge are shown in Table 1.
TABLE 1 moisture content and repeatability in titanium sponge
Through multiple measurement experiments, the inventors found that: the sponge titanium samples with different particle diameters are measured, the relative error is within 10%, and the precision of moisture content detection is good; taking 1g of a titanium sponge sample with the particle size ranging from 1.10 cm to 1.50cm for testing, and carrying out a test on 200mL of the maximum extractant dioxane, wherein the detection limit is calculated to be 10mg/kg; titanium sponge samples with particle sizes ranging from 1.10 cm to 1.50cm were placed at room temperature at 25℃and in an environment with humidity of 10% and 50% respectively for 10 hours, and the water contents were determined to be 120mg/kg and 258mg/kg, respectively. Indicating that the titanium sponge water absorption is related to the ambient humidity; titanium sponge samples with particle sizes ranging from 1.10 cm to 1.50cm were placed at room temperature at 25℃and humidity at 50% for 2 hours and 10 hours, and their water contents were determined to be 125mg/kg and 260mg/kg, respectively. Indicating that the water absorption of titanium sponge is related to the time of placement in the environment.
Claims (5)
1. The method for measuring the moisture content in the titanium sponge is characterized by comprising the following steps of:
s1, sample preparation: preparing a sample with the particle size ranging from 0.1cm to 6cm from titanium sponge, and grouping the sample according to different particle sizes by using a classifying screen;
s2, preparation of an extract: weighing 1g-20g from a group of samples, placing the samples into a wide-mouth bottle, weighing until the sample is 0.0002 and g, covering the wide-mouth bottle with a rubber stopper, injecting 50.0-200.0mL of organic extractant into the wide-mouth bottle by using a syringe, placing the wide-mouth bottle in an ultrasonic cleaner for cleaning for 30 min, standing for 15min, shaking or oscillating until the sample solution is uniform, taking part of the solution to be placed in a centrifuge tube with the rubber stopper for centrifugation after the sample is slightly settled, and taking the centrifugate as an extract for standby;
s3, determination: calculating the moisture content in the group of sample extracts by Fischer titration measurement;
s4, repeating the steps S1-S3 to obtain the moisture content of each group of samples, taking the weights of the samples of different groups as weights, and calculating a weighted average value to obtain the moisture content of the titanium sponge product.
2. The method for measuring the moisture content in titanium sponge according to claim 1, wherein the method comprises the steps of: step S1, preparing a sample with the particle size ranging from 0.1cm to 3cm from the titanium sponge, and classifying the sample into six groups according to the particle size of 0.10 to 0.50cm,0.51 to 1.00cm,1.10 to 1.50cm,1.51 to 2.00cm,2.01 to 2.50cm and 2.51 to 3.0 cm by using a classifying screen.
3. The method for measuring the moisture content in titanium sponge according to claim 1 or 2, characterized by comprising the steps of: the organic extractant in the step S2 is any one of dioxane, absolute ethyl alcohol and methanol.
4. The method for measuring the moisture content in titanium sponge according to claim 3, wherein: step S2, 1g of the sample is weighed out and placed in a 500mL wide-mouth bottle, and 200.0mL of the organic extractant is dioxane by using a syringe.
5. The method for measuring the moisture content in titanium sponge according to claim 4, wherein the method comprises the steps of: the detection limit of the measuring method is 10mg/kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311250216.9A CN117288886A (en) | 2023-09-26 | 2023-09-26 | Method for measuring moisture content in titanium sponge |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202311250216.9A CN117288886A (en) | 2023-09-26 | 2023-09-26 | Method for measuring moisture content in titanium sponge |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN117288886A true CN117288886A (en) | 2023-12-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202311250216.9A Pending CN117288886A (en) | 2023-09-26 | 2023-09-26 | Method for measuring moisture content in titanium sponge |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN117288886A (en) |
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2023
- 2023-09-26 CN CN202311250216.9A patent/CN117288886A/en active Pending
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