CN102507484A - Method for measuring content of zinc in compound montmorillonite preparation - Google Patents
Method for measuring content of zinc in compound montmorillonite preparation Download PDFInfo
- Publication number
- CN102507484A CN102507484A CN2011103102431A CN201110310243A CN102507484A CN 102507484 A CN102507484 A CN 102507484A CN 2011103102431 A CN2011103102431 A CN 2011103102431A CN 201110310243 A CN201110310243 A CN 201110310243A CN 102507484 A CN102507484 A CN 102507484A
- Authority
- CN
- China
- Prior art keywords
- zinc
- smectite
- sample
- preparation
- compound
- 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
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a method for measuring the content of zinc in a compound montmorillonite preparation, comprising the following steps: breaking the crystal structure of montmorillonite by using a right method so that the montmorillonite can not absorb zinc ions, dissolving out all the zinc by using acid, measuring the absorbance of a reference solution and a sample solution by adopting the atomic absorption spectrophotometry, and calculating the content of the zinc in a sample.
Description
Technical field
The present invention relates to the content assaying method of zinc in a kind of compound smectite, specifically is to use atomic absorption spectrophotometry.
Background technology
The compound smectite is to be processed by smectite, the medicinal raw material that contains zinc and pharmaceutic adjuvant, and the compound smectite is a medical product, need measure the content of zinc, to guarantee the quality of medicine.Zinc ion can produce exchange with calcium, the sodium in the smectite in water; Water can not be with zinc stripping fully from sample; With ammonium chloride-ethanol exchange liquid can be with the complete stripping of zinc; But in the liquid of stripping, also contain calcium ion simultaneously, can produce bigger error, cause the mensuration result inaccurate with EDTA complexometric titration zinc.
Summary of the invention
The purpose of this invention is to provide a kind of accurately, the content assaying method of zinc in reliable, the compound smectite that specificity is strong, in order to guarantee the quality of compound smectite.
Method of the present invention realizes through following technical scheme.
1, the processing of sample:
Destroy the crystal structure of smectite earlier with appropriate method, make it not produce suction-operated, make all strippings of zinc zinc ion.Method has and comprises: sample is with sulfuric acid and nitric acid or with sodium carbonate and soda mint heating; The sample heating adds sulfuric acid and ethanol, the heating of repeated hydrogenation fluoric acid; Sample adds anhydrous lithium metaborate heating.Zinc solubleness in sour water is big, thus use the sour water stripping, and the washing residue, make the zinc stripping complete, again thin up, constant volume.
2, atomic absorption spectroscopy determination:
Get the solution of above-mentioned preparation, the photograph atomic absorption spectrophotometry (" two appendix IV of Chinese pharmacopoeia version in 2010 D, first method), measure in the wavelength of 213.9nm.
Use flame atomizer stone or black stove atomizer in the atomic absorption spectrophotometry method of the present invention.Determination method adopts calibration curve method, measures the zinc reference substance solution, and the drawing standard curve is measured need testing solution, calculates content.
The inventive method is through methodological study; The result shows that zinc is that 0.05 μ g/ml～0.4 μ g/ml scope internal linear relation is good in concentration; R=0.9999, need testing solution is 0.982% at 8 hours RSD of room temperature, replica test RSD as a result is 1.337%; It is 1.25% that date precision is measured RSD, and it is 1.19% that personnel's precision is measured RSD.Above each item result shows that this method is accurate, stable, reliable.
Embodiment
Below in conjunction with embodiment the present invention is further described
Embodiment 1:
Get the zinc standard solution, thin up is processed and is contained the solution that zinc is respectively 0.05 μ g, 0.1 μ g, 0.2 μ g, 0.3 μ g, 0.4 μ g among every 1ml approximately, as reference substance solution.
Sample mix is even, gets 1.3g, and accurate the title decides, and puts in the porcelain dish, adds sulfuric acid 6ml and nitric acid 10ml respectively; Treat effect fully, put evaporate to dryness in the sand bath, put coldly, add dilute sulfuric acid (9.5%-10.5%) 30ml; Boil, upper strata liquid filters through ashless filter paper with decantation, and with hot wash 3 times, filtrating merges residue with decantation; Put in the 100ml measuring bottle, put and be chilled to room temperature, thin up shakes up to scale.Precision is measured 5ml and is put in the 50ml measuring bottle, and thin up shakes up to scale, and precision is measured 5ml and put in the 50ml measuring bottle, and thin up shakes up as need testing solution to scale.
Get reference substance solution and need testing solution and measure absorbance, the content of zinc in the calculation sample.
Embodiment 2:
Get the zinc standard solution, thin up is processed and is contained the solution that zinc is respectively 0.05 μ g, 0.1 μ g, 0.2 μ g, 0.3 μ g, 0.4 μ g among every 1ml approximately, as reference substance solution.
Sample mix is even, gets 0.5g, and accurate the title decides, and puts in the platinum crucible; Add 0.5g sodium carbonate and the 0.5g soda mint stirs, be heated to 800 ℃ and kept 3 hours, cooling, gradation add dilute sulfuric acid (9.5%-10.5%) 50ml altogether; Stirring makes the residue dissolving and transfers in the 250ml measuring bottle, and thin up shakes up to scale; Precision is measured 5ml and is put in the 50ml measuring bottle, and thin up shakes up as need testing solution to scale.
Get reference substance solution and need testing solution and measure absorbance, the content of zinc in the calculation sample.
Embodiment 3:
Get the zinc standard solution, thin up is processed and is contained the solution that zinc is respectively 0.05 μ g, 0.1 μ g, 0.2 μ g, 0.3 μ g, 0.4 μ g among every 1ml approximately, as reference substance solution.
Sample mix is even, gets 0.25g, and accurate the title decides, and puts in the platinum crucible; Be heated to 900 ℃ and kept 2 hours, cooling adds sulfuric acid 0.2ml and 2ml ethanol, makes sample moistening; Add hydrofluorite 61ml heating, be heated to 100-300 ℃ and be evaporated to gas and eliminate, cooling, gradation add dilute sulfuric acid (9.5%-10.5%) 50ml altogether; Stirring makes the residue dissolving and transfers in the 250ml measuring bottle, and thin up shakes up to scale; Precision is measured 2ml and is put in the 50ml measuring bottle, and thin up shakes up as need testing solution to scale.
Get reference substance solution and need testing solution and measure absorbance, the content of zinc in the calculation sample.
Sample mix is even, gets 0.25g, and accurate the title decides, and puts in the platinum crucible, adds anhydrous lithium metaborate 1g; Mixing is heated to 1100 ℃, keeps 15 minutes; Cooling, gradation add dilute sulfuric acid (9.5%-10.5%) 50ml altogether, and stirring makes the residue dissolving and transfers in the 250ml measuring bottle, and thin up is to scale; Shake up, precision is measured 2ml and is put in the 50ml measuring bottle, and thin up shakes up as need testing solution to scale.
Get reference substance solution and need testing solution and measure absorbance, the content of zinc in the calculation sample.
Claims (7)
1. the assay method of zinc is characterized in that in the compound smectite preparation:
1) sample preparation is destroyed the crystal structure of smectite earlier, and method has sample to heat with sulfuric acid and nitric acid or with sodium carbonate and soda mint heating or sample heating, adds sulfuric acid and ethanol, and heating of repeated hydrogenation fluoric acid or sample add anhydrous lithium metaborate heating;
2) after the sample preparation, with sour water stripping zinc;
3) get reference substance solution and need testing solution is measured absorbance with atomic absorption spectroscopy determination, the content of zinc in the calculation sample.
2. the assay method according to zinc in the said compound smectite of claim 1 preparation is characterized in that: destroy the crystal structure of smectite, method is that sample is put in the porcelain dish, adds sulfuric acid and nitre respectively, and the effect of treating fully, is put evaporate to dryness in the sand bath, puts cold.
3. the assay method according to zinc in the said compound smectite of claim 1 preparation is characterized in that: destroy the crystal structure of smectite, method is that sample is put in the platinum crucible, adds sodium carbonate with soda mint stirs, and is heated to 800 ℃ and keeps 3 hours, cools off.
4. the assay method according to zinc in the said compound smectite of claim 1 preparation is characterized in that: destroy the crystal structure of smectite, method is that sample is put in the platinum crucible, is heated to 900 ℃ and keeps 2 hours; Cooling; Add sulfuric acid and ethanol, make sample moistening, add the hydrofluorite heating; Be heated to 100-300 ℃ and be evaporated to gas and eliminate, cooling.
5. the assay method according to zinc in the said compound smectite of claim 1 preparation is characterized in that: destroy the crystal structure of smectite, method is that sample adds anhydrous lithium metaborate, and mixing is heated to 1100 ℃, keep, and 15 minutes, cooling.
6. the assay method according to zinc in the said compound smectite of claim 1 preparation is characterized in that: the mensuration wavelength is 213.9nm.
7. the assay method according to zinc in the said compound smectite of claim 1 preparation is characterized in that: sour water is a dilute sulfuric acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103102431A CN102507484A (en) | 2011-10-14 | 2011-10-14 | Method for measuring content of zinc in compound montmorillonite preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103102431A CN102507484A (en) | 2011-10-14 | 2011-10-14 | Method for measuring content of zinc in compound montmorillonite preparation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102507484A true CN102507484A (en) | 2012-06-20 |
Family
ID=46219591
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103102431A Pending CN102507484A (en) | 2011-10-14 | 2011-10-14 | Method for measuring content of zinc in compound montmorillonite preparation |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102507484A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106979945A (en) * | 2017-04-24 | 2017-07-25 | 重庆长安工业(集团)有限责任公司 | A kind of method of Zn content in measure zincizing agent |
| CN108152096A (en) * | 2017-11-28 | 2018-06-12 | 广东南芯医疗科技有限公司 | A kind of method that tellurium selenium cobalt ions in human faecal mass is removed using lithium base chlorite |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101477068A (en) * | 2009-01-20 | 2009-07-08 | 济南康众医药科技开发有限公司 | Medicinal smectite content measuring standard |
-
2011
- 2011-10-14 CN CN2011103102431A patent/CN102507484A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101477068A (en) * | 2009-01-20 | 2009-07-08 | 济南康众医药科技开发有限公司 | Medicinal smectite content measuring standard |
Non-Patent Citations (2)
| Title |
|---|
| 刘静静等: "国内膨润土防水毯行业存在的若干问题及对策", 《中国非金属矿工业导刊》 * |
| 尚宏芳等: "滴定法测定蒙脱石散中三氧化二铝的含量", 《黑龙江医药》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106979945A (en) * | 2017-04-24 | 2017-07-25 | 重庆长安工业(集团)有限责任公司 | A kind of method of Zn content in measure zincizing agent |
| CN108152096A (en) * | 2017-11-28 | 2018-06-12 | 广东南芯医疗科技有限公司 | A kind of method that tellurium selenium cobalt ions in human faecal mass is removed using lithium base chlorite |
| CN108152096B (en) * | 2017-11-28 | 2020-08-25 | 广东南芯医疗科技有限公司 | Method for removing tellurium, selenium and cobalt ions in human excrement by utilizing lithium-based chlorite |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Skidmore et al. | The determination of esterified fatty acids in glycerides, cholesterol esters, and phosphatides | |
| Garratt | The quantitative analysis of drugs | |
| CN103884676B (en) | A kind of rapid assay methods of Chinese crude drug multi-target ingredient content | |
| Akramipour et al. | Development of an efficient sample preparation method for the speciation of Se (IV)/Se (VI) and total inorganic selenium in blood of children with acute leukemia | |
| CN102507484A (en) | Method for measuring content of zinc in compound montmorillonite preparation | |
| CN108802250A (en) | The method that ultra high efficiency LC-MS detects 11 kinds of neurotransmitters in encephalic micro-dialysis liquid | |
| CN102879495A (en) | Antidotal capsule of Tibetan medicine compound and quality detection method of preparation of antidotal capsule | |
| CN101477068A (en) | Medicinal smectite content measuring standard | |
| CN102841176B (en) | Zhenlong xingnao (Chinese character) capsule of Tibetan medicine composition and detection method of iron content in preparation thereof | |
| CN102809542A (en) | Determination method of polysaccharide content of rhodiola rosea injection | |
| CN112505175B (en) | Method for determining content of impurities in peritoneal dialysis solution | |
| CN104833756B (en) | A kind of content assaying method of attached sweet medicine monoester alkaloid | |
| CN102841094B (en) | Method for determining ferrous powder content of Tibetan medicine decoction pieces in traditional Chinese medicine preparation | |
| CN104458369B (en) | A kind of preparation method of plasma spectroscopy detection titanium oxide solution sample | |
| Filatova et al. | Determination of gallium in biological fluids using inductively coupled plasma mass spectrometry | |
| CN102841095B (en) | Quality testing method for Liuwei Mingmu preparation of Tibetan medicine composition | |
| CN108107038A (en) | A kind of method of total alkaloid constituents dissolution rate in quick detection Summer interplanting cotton | |
| CN107340291A (en) | A kind of content of formaldehyde assay method | |
| Desai et al. | A new polarimeteric method for the analysis of sucrose-in iron sucrose raw material, iron sucrose injection and inprocess bulk formulations | |
| CN102670887B (en) | Method for processing rhizoma arisaematis | |
| CN102379894B (en) | Content determination method for montmorillonite preparation | |
| CN102879389B (en) | Liver tonifying, blood activating and eyesight improving pill of Tibetan medicine compound and quality detection method of preparation of pill | |
| CN108333135A (en) | The analysis method of Norfloxacin content in a kind of norfloxacin capsule | |
| Chen | Generation mechanisms of hydrogen cyanide and ammonia in human exhaled breath | |
| CN109358151B (en) | Thin-layer chromatography detection method for 1, 4-butanediamine impurity in L-2-amino-5-guanidino valeric acid raw material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120620 |