An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method（HPCD）, is stud...An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method（HPCD）, is studied by an inductively coupled plasma optical emission spectrometry（ICP-OES） and an inductively coupled plasma mass spectrometry（ICP-MS）. The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error（RE） for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials（GBW07309, GBW07311, GBW07313）, rock reference materials（GBW07103, GBW07104,GBW07105）, and cobalt-rich crust reference materials（GBW07337, GBW07338, GBW07339）, the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation（RSD） and the relative error（RE） are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.展开更多
By analyzing heat transfer on the wall of fiat steel ribbon wound vessel （FSRWV）, a numerical model of temperature distribution on the entire wall （including inner core wall, flat steel ribbons, outside cylinder of...By analyzing heat transfer on the wall of fiat steel ribbon wound vessel （FSRWV）, a numerical model of temperature distribution on the entire wall （including inner core wall, flat steel ribbons, outside cylinder of jacket and insulating layer） was established by the authors. With the model, the temperature distribution and the length change in the vessel walls and flat steel ribbons in low temperature are calculated and analyzed. The results show that the flat steel ribbon wound cryogenic high-pressure vessel is simpler in structure, safer and easier to manufacture than those of conventional ones.展开更多
基金The China Ocean Mineral Resources Research and Development Association Research Program of the State Oceanic Administration of China under contract No.DY125-13-R-07the National Natural Science Foundation of China under contract Nos 41322036 and 41230960+1 种基金the Shandong Provincial Natural Science Foundation of China under contract No.ZR2014DP009the Special Basic Research Funds for Central Public Research Institutes for The First Institute of Oceanography,State Oceanic Administration of China under contract Nos GY0213G06 and GY02-2012G35
文摘An improved analytical method to determine the content of 52 major, minor and trace elements in marine geological samples, using a HF-HCl-HNO_3 acid system with a high-pressure closed digestion method（HPCD）, is studied by an inductively coupled plasma optical emission spectrometry（ICP-OES） and an inductively coupled plasma mass spectrometry（ICP-MS）. The operating parameters of the instruments are optimized, and the optimal analytical parameters are determined. The influences of optical spectrum and mass spectrum interferences, digestion methods and acid systems on the analytical results are investigated. The optimal spectral lines and isotopes are chosen, and internal standard element of rhodium is selected to compensate for matrix effects and analytical signals drifting. Compared with the methods of an electric heating plate digestion and a microwave digestion, a high-pressure closed digestion method is optimized with less acid, complete digestion,less damage for digestion process. The marine geological samples are dissolved completely by a HF-HCl-HNO_3 system, the relative error（RE） for the analytical results are all less than 6.0%. The method detection limits are 2–40μg/g by the ICP-OES, and 6–80 ng/g by ICP-MS. The methods are used to determine the marine sediment reference materials（GBW07309, GBW07311, GBW07313）, rock reference materials（GBW07103, GBW07104,GBW07105）, and cobalt-rich crust reference materials（GBW07337, GBW07338, GBW07339）, the obtained analytical results are in agreement with the certified values, and both of the relative standard deviation（RSD） and the relative error（RE） are less than 6.0%. The analytical method meets the requirements for determining 52 elements contents of bulk marine geological samples.
文摘By analyzing heat transfer on the wall of fiat steel ribbon wound vessel （FSRWV）, a numerical model of temperature distribution on the entire wall （including inner core wall, flat steel ribbons, outside cylinder of jacket and insulating layer） was established by the authors. With the model, the temperature distribution and the length change in the vessel walls and flat steel ribbons in low temperature are calculated and analyzed. The results show that the flat steel ribbon wound cryogenic high-pressure vessel is simpler in structure, safer and easier to manufacture than those of conventional ones.
文摘目的探讨长期甲醛固定的大鼠视网膜胰蛋白酶消化的最佳消化时间和最佳胰蛋白酶浓度。方法健康♂ SD大鼠，颈椎脱臼处死，摘取眼球，放入4％甲醛固定液，固定时间为2 d、2周、4周、3月、5月、7月。分离固定不同时间的视网膜，放入3％、6％、9％胰蛋白酶消化，37℃恒温箱孵育。分别记录固定不同时间的视网膜在3％、6％、9％胰蛋白酶中消化完全所需时间。铺片操作，行 PAS 染色。显微镜下记录视网膜消化情况。结果新鲜眼球常规固定48 h，3％胰蛋白酶37℃消化3.5 h，视网膜消化完全。对于甲醛固定2周及1月的大鼠眼球，采用常规胰蛋白酶浓度（3％），仅延长胰蛋白酶的消化时间至9 h 及14 h，可以达到常规固定组织的消化效果。对于固定3月的大鼠眼球，采用常规浓度的胰蛋白酶仅延长消化时间至22 h，同样可以得到完整的视网膜血管铺片，且提高胰蛋白酶浓度对于缩短视网膜消化时间的影响不大。而对于固定5～7月的大鼠眼球，6％和9％浓度的胰蛋白酶可以在一定程度上缩短视网膜消化的时间至22 h 和28 h，有利于得到相对完整的视网膜血管。结论固定时间短于3月的眼球组织，采用3％胰蛋白酶消化，延长消化时间可达到最佳消化效果。对于固定5～7月的视网膜组织，不仅需要延长消化时间，还需要通过提高胰蛋白酶浓度至6％，才可以获得最佳消化效果的视网膜血管。
