原子吸收法测定Fe—Co—V合金中锰,镍,铜

介绍用火焰原子吸收光主普法同时测定Ｆｅ－Ｃｏ－Ｖ合金中锰、镍、铜的含量,研究了实验条件及影响因素,建立了有效的分析方法,结果表明,锰、镍、铜含量在０．５～５．０ｍｇ．Ｌ＾－１范围的回收率为９７％～１０３％,ＲＳＤ〈３．０％（ｎ＝１０）,具有良好的准确性和重现性。     

电位滴定法连续测定钴、镍和铜的方法研究（Ⅱ）

本文以Ｐｔ电极作指示电极,Ｗ电极作参比电极,在氨性介质中,以Ｋ＿３Ｆｅ（ＣＮ）＿６滴定Ｃｏ￣（２＋）以后,继而利用Ｆｅ（ＣＮ）／Ｆｅ（ＣＮ）作指示离子,在ｐＨ５．５～６．０,用Ｚｎ￣（２＋）返滴定ＥＤＴＡ,连续测定Ｎｉ￣（２＋）或Ｎｉ￣－Ｃｕ含量,再用硫酸肼作Ｃｕｙ￣（２－）的释放剂,Ｚｎ￣（２＋）返滴定释放出的ＥＤＴＡ测定Ｃｕ￣（２＋）,实现了Ｃｏ－Ｎｉ－Ｃｕ连续测定。镍精矿样分析的相对标准偏差和试样中标准回收率分别为Ｃｏ：１．４％,９９．５±１．２％。Ｎｉ：１．１％,１００．１±０．９％。Ｃｕ：２．０     

火焰原子吸收光谱法快速测定纯镍中铁铜镁锰锌

提出了运用火焰原子吸收光谱法快速测定纯镍中铁铜镁锰锌的含量，介绍了铁铜镁锰锌最佳测定条件及呈良好线性范围的浓度，在测定中对样品中的干扰因素进行了综合考虑。该方法具有很好的灵敏度和重现性，具有方法步骤简单、操作容易、干扰少等特点。测定样品铁铜镁锰锌含量的相对标准偏差均小于1．0％（n=10）。标准加入回收率均在97．0％～99．0％（n=6）范围内。适用于纯镍材料中铁铜镁锰锌的含量控制分析和系统分析。     

硫化镍铜多金属共生贫矿石的浮选

超基性岩型硫化镍铜多金属共生贫矿石中矿物种类繁多，嵌镶关系复杂，伴生有价金属丰富。该矿石的分选，尤其是精矿降镁难度大。采用以ＡＳ－４为捕收起泡剂分速浮选，中矿添加ＡＴ－４、ＡＴ－５等调整剂集中再选的ＢＦＰ全混合浮选工艺，获得了良好的选别指标，原矿镍品位０．６０％，铜品位０．３９％时，镍铜混合精矿含镍６．７４％，含铜４．５５％，含氧化镁５．９０％，含钴０．１７％，镍回收率７３．３２％，铜回收率７５．     

ICP—AES法测定LiCoO2中杂质成分的分析方法研究

研究建立了电感耦合等离子发射光谱（ＩＣＰ－ＡＥＳ）法测定锂离子电池电极材料中杂质成份镍、钠、钙的分析方法。试样分析与误差统计结果分别为：相对标准偏差（ＲＳＤ）（ｎ＝６）;镍≤４．４％,钠≤８．５％、钙≤４．６％,加标回收率;镍９８．３％～１０１．３％,铁９９．６％～１０２．５％、钠９９．６％～１０２．５％、钙９６．０％～１０％。该分析方法准确、简便、快速,完全能满足锂离子电池有材料分析的要求。     

钼（Ⅳ）─3，5─diBr─PADAP─盐酸羟胺多元混配体系显色反应的研究及其分析应用

在ｐＨ２．４～３．５的酸性介质中及加热条件下,钼（ＶＩ）与２－（３,５一二溴－２－吡啶偶氮）－５－二乙氨基苯酚（３,５－ｄｉＢｒ－ＰＡＤＡＰ）及羟胺反应形成一种稳定的蓝色络合物,组成比为１：１：１。在十二烷基硫酸钠存在下,其最大吸收波长为６ｌ８ｎｍ,表现摩尔吸光系数为４．８×ｌ０￣４,钼含量在０～２５μｇ／１０ｍｌ时服从比尔定律。毫克量钨无干扰。铜、钴、镍、铁等高厂的干扰可通过离厂交换分离除去。本法用于测定软磁合金中的铝,获得了满意的结果。     

2－（3，5－二氯－2－吡啶偶氮）－5－二甲氨基苯胺与铜（Ⅱ）反应的分光光度研究及其应用

研究了２－（３,５－二氯２－吡啶偶氮）－５－二甲氨基苯胺与铜（Ⅱ）的反应事件。在ｐＨ３．５～４．５范围内,试剂与铜（Ⅱ）形成１：１的稳定配合物,其最大吸收波长为５８６ｎｍ,表观摩尔吸光系数为５．４５×１０￣。铜（Ⅱ）浓度在０～２４μｇ／２５ｍｌ范围内符合比尔定律。方法简便、快速、选择性好,利于铝合金中微量铜的测定,结果满意。     

锰含量与钢性能的关系

锰含量与钢性能的关系金属元素锰对钢的性能影响较大，按照含锰量的不同碳素钢可分为普通含锰量（０．２５％～０．８０％Ｍｎ）和较高含量锰（０．７％～１．２％Ｍｎ）两组，其性能也不相同。含锰量小于０．２％的钢材，锰是以杂质形式存在于钢中，它具有使钢脱氧、脱硫...     

Rhod 6G－BiIn－SDS＋Triton X－200体系的形成机理与应用

研究了Ｒｈｏｄ６Ｇ－ＢｉＩｎ－ＳＤＳ＋ＴｒｉｔｏｎＸ－２００体系的形成机理与应用。ＳＤＳ＋ＴｒｉｔｏｎＸ－２００与配体Ｒｈｏｄ６Ｇ形成混合胶团，对显色体系产生增溶、增敏作用，实现了缔合物的水相测定。在ｐＨ为１．８时，试剂空白的λｍａｘ为５３１ｎｍ，缔合物的λｍａｘ为５８０ｎｍ，△λ为４９ｎｍ。在含铋０～８．０μｇ／２５ｍＬ的范围内符合比尔定律，表现摩尔吸收系数ε为３．４６×１０５Ｌ／（ｍｏｌ·ｃｍ）。该体系选择性好，可不经分离直接用于测定铋含量均超过０．００１％的铁、精密合金、铜小于０．５％，镍小于４％，钨小于３％的合金钢和高温合金。     

邻硝基苯基荧酮光度法测定矾土中镁

在硼砂－ＮａＯＨ（ｐＨ１０．５）缓冲溶液中,当ＣＰＢ和ＯＰ存在,邻硝基苯基荧光酮与镁（Ⅱ）显色,λｍａｘ＝６１０ｎｍ,镁量在０～０２μｇ／５０ｍＬ范围内符合比尔定律。用环已烷二胺四乙酸钙－三乙醇胺－四乙烯五胺混合液,掩蔽铝、铁、钛、锰和重金属离子的干扰,可用于钒土中０．０５％～１．００％镁的测定。     

二乙基三胺五乙酸浸取-电感耦合等离子体质谱法测定石灰性土壤中有效态铜锌铁锰

采用二乙基三胺五乙酸(DTPA)浸提石灰性土壤样品中有效态Cu、Zn、Fe、Mn后,样品溶液基体盐分较大,此时若直接采用电感耦合等离子体质谱法(ICP-MS)进行测定,极易使仪器的采样锥和截取锥发生堵塞,雾室和炬管积盐,进而影响测定准确性。据此,实验用DTPA浸提样品后,采用对样品溶液稀释10~30倍和在标准溶液系列中加入DTPA溶液进行基体匹配的方法以消除基体干扰,利用氦碰撞模式进行测定以消除多原子离子⁴⁰Ar¹⁶O对⁵⁶Fe的质谱干扰,最终实现了ICP-MS对石灰性土壤中有效态Cu、Zn、Fe、Mn的测定。对氦气流量进行了优化,并确定氦气流量为4.5mL/min。在优化的实验条件下,Cu、Zn的质量浓度为5~200ng/mL、Fe的质量浓度为100~3000ng/mL、Mn的质量浓度为30~1000ng/mL时,各元素质量浓度分别与其计数值呈线性关系,相关系数均不小于0.9998。方法检出限为0.003~0.01mg/kg。按照实验方法测定土壤有效态成分分析标准物质中的有效态Cu、Zn、Fe、Mn,测定值与认定值一致,相对标准偏差(RSD)为1.3%~3.1%。采用实验方法和标准方法HJ 804—2016(电感耦合等离子体原子发射光谱法)进行方法对照试验,二者测定值基本一致。     

电感耦合等离子体原子发射光谱法测定铌锰铁中铌和锰

铌锰铁是炼钢过程中的一种重要原料,建立测定铌和锰的方法尤为重要。铌锰铁中铌和锰为主元素,含量高,运用化学湿法分析时主元素之间会相互干扰,影响测定的准确性。实验采用盐酸、硝酸、氢氟酸溶解样品,选择Nb 269.706nm为分析线、Mo 281.618nm为内标线;选择Mn 293.305nm为分析线、V 292.401nm为内标线,建立了采用电感耦合等离子体原子发射光谱法(ICP-AES)测定铌锰铁中铌和锰的方法。共存元素的干扰校正试验表明,样品中共存元素对待测元素无干扰。各待测元素的校准曲线线性相关系数均大于0.9995。实验方法用于铌锰铁实际样品中铌和锰的测定,铌测定结果的相对标准偏差(RSD,n=11)为0.26%~0.28%;锰测定结果的相对标准偏差(RSD,n=11)为0.29%~0.33%。采用实验方法对铌锰铁实际样品中铌和锰进行测定,测得结果分别与日本标准JIS G 1328—1982中丹宁酸水解重量法测定铌和国标GB/T 5686.1—2008中高氯酸氧化滴定法测定锰的结果基本一致。     

Iron stores and coagulation parameters in patients with hypoxemic polycythemia secondary to chronic obstructive pulmonary disease: the effect of phlebotomies

This study was designed to determine the effects of phlebotomy on iron body contents and coagulation tests of COPD patients with polycythemia secondary to hypoxemia. Seventeen patients with COPD and hematocrits higher than 54 percent (mean Hct: 57 +/- 0.49 percent), who had not received anti-inflammatory or antiplatelet aggregation agents recently. Their mean forced expiratory volume at 1 second (FEV1) was 0.92 +/- 0.11 L. Intervention: Blood work was collected to evaluate the following: serum iron and ferritin levels, total iron binding capacity, transferrin saturation index, fibrinogen plasma levels, activated partial thromboplastin time, platelet count, platelet aggregation measurements, and thromboelastography coagulation parameters. The blood samples were obtained before and about 7 days after the hematocrit correction by 300-400 ml phlebotomies done every other day. The mean number of phlebotomies done for each patient was 4.4. Postphlebotomy iron serum levels decreased from 90.1 +/- 14.8 to 59.7 +/- 9.9 mg/dl and the ferritin serum levels from 133.8 +/- 37.9 to 70.8 +/- 32.7 ng/ml (p < 0.05). Regarding the coagulation studies, there were significant increases in the platelet count, from 227,300 +/- 13,900 to 312,500 +/- 30,200 per mm3, and in the maximum clot amplitude (a) obtained by thromboelastography (from 53.6 +/- 1.4 percent to 60.4 +/- 1.1 percent). The coagulation time (k) of the thromboelastography also decreased significantly, from 7.5 +/- 0.7mm prephlebotomy to 4.5 +/- 0.3mm postphlebotomy. Although the coagulation changes were small amount, the observed significant decrease in iron contents may have clinical implications.     

Variability in estimation of coronary dimensions from 6F and 8F catheters

To investigate the suitability of diagnostic 6F catheters for coronary angiographic measures in the clinical setting, we determined the relative accuracy and reproducibility of the measures obtained with these catheters as scaling devices in 59 stenoses. Comparison was made with duplicate injections, obtained before angioplasty, using an 8F guiding catheter as scaling device. Intra- and interobserver variability was evaluated in 15 stenoses. The coefficient of variation averaged 18.3% for the minimal lumen diameter, 10.4% for the percent stenosis, and only 7.4% for the reference diameter. Reproducibility of angiographic measures done with the 6F catheter was similar to that obtained with the 8F catheter, although accuracy was lower with the 6F for the measurement of reference diameter. Thus, quantitative coronary angiography (QCA) measures derived from routine diagnostic angiograms may be suitable for determination of reference diameter, allowing enough precision for determination of the size of a coronary device for intervention, but these measures may lack accuracy for precise determination of minimum diameter and percent stenosis, making their use questionable in studies looking at individual changes in coronary stenosis dimensions.     

Sensitivity of monoclonal antibodies to carcinoembryonic antigen, tissue polypeptide antigen, alpha-fetoprotein, carbohydrate antigen 50, and carbohydrate antigen 19-9 in the diagnosis of colorectal adenocarcinoma

PURPOSE: This study was designed to establish the sensitivity of monoclonal antibodies to carcinoembryonic antigen (CEA), alpha-fetoprotein (AFP), tissue polypeptide antigen (TPA), carbohydrate antigen 50 (CA 50), and carbohydrate antigen 19-9 (CA 19-9) and the efficacy of the joint determination of several tumor markers, as well as the dynamics of postoperative normalization of each marker in the absence of recurrence. MATERIALS AND METHODS: A prospective study was carried out in 100 patients subjected to surgical resection of colon adenocarcinoma. Serum concentrations of these markers were determined the day before surgery and seven days, two months, and six months after surgery. RESULTS: The results demonstrate that sensitivity increased as the disease spread and that CA 19-9 was the most sensitive tumor marker. The rate of false negatives was 40 percent for Dukes Stage A lesions, 19 percent for Dukes Stage B, 7 percent for Dukes Stage C, and 0 percent for Dukes Stage D. Determination of two markers (CA 19-9 and CEA) provided the greatest sensitivity in Stages A and D tumors (60 percent and 100 percent, respectively); the incidence did not change when measurements of other antigens were associated. For Stages B and C, determination of at least three markers was necessary, the association of CEA, TPA, and CA 19-9 being that which showed the greatest sensitivity, 78 percent and 91 percent, respectively. CONCLUSIONS: It would be advisable to include monoclonal antibody determination of CEA, TPA, and CA 19-9 in the diagnosis of adenocarcinoma, despite the fact that ultimate sensitivity will depend on the degree of tumor extension or on the presence of metastasis.     

X射线荧光光谱法在鹿鸣矿业钼选矿流程中的应用

采用粉末压片法制样,建立了X射线荧光光谱仪快速测定鹿鸣矿业钼选矿流程中的原矿、尾矿、快浮尾矿中Mo、Cu、S等3种元素的分析方法。由于钼矿石标准样品较少,因此实验选取钼选矿流程中不同阶段且含量呈梯度的多个经湿法准确定值的样品作为校准样品建立校准曲线。将样品研磨至0.074mm以下,采用经验系数法校正元素间的影响,消除基体效应、粒度效应,降低谱线重叠干扰。各元素的检出限在3~10μg/g之间,各组分测定结果的相对标准偏差(RSD)在0~5.1%之间。对钼选矿流程中原矿、尾矿、快浮尾矿样品进行正确度考察,测定值与湿法值一致。分别选取流程中原矿、尾矿、快浮尾矿样品在不同时间进行长期稳定性考察,3个元素测定结果的相对标准偏差在0.18%~7.9%之间。     

惰气熔融-热导/红外法测定钛合金中氧氮氢

钛合金中氧、氮和氢的含量对其力学性能影响很大,因此,需要对其准确测定.采用氢氟酸和硝酸体积比为1∶3的酸洗液清洗样品后再用无水乙醇浸泡的方法处理样品,测氧和氮时样品质量选择0.10g,测氢时样品质量选择0.20g,以镍篮为助熔剂,实现了惰气熔融-热导/红外法对钛合金中氧、氮和氢的测定.试验表明,样品放置4h与放置1d,...     

高频感应燃烧红外吸收法测定焊接药剂中硫含量

研究了高频感应燃烧红外吸收法测定焊剂、焊条药皮和药芯焊丝药粉等焊接药剂中硫含量的方法。最佳工作条件为先将0.1~0.15g样品加入预先放置有0.3~0.5g铁屑的瓷坩埚中,再覆盖0.2g锡粒和1.7g钨粒;采用0.3~0.5g钢铁有证标准样品建立校准曲线(助熔剂为0.2g锡粒-1.7g钨粒)。结果表明,方法的测定下限为0.005%(高纯氧气)至0.008%(普通氧气)。将实验方法用于不同硫含量的焊接药剂实际样品的分析,结果的相对标准偏差(RSD,n=6)不大于7%,加标回收率为83%~107%。采用焊剂及矿石标准样品进行准确度验证,测定值与认定值相符合。     

自动电位滴定法测定锰矿石中全锰量

样品经盐酸、磷酸、硝酸、高氯酸加热溶解后,采用自动电位滴定法测定全锰量。经过对5个有证标准样品进行测试,测定的平均值与标准值的误差在0.015%～0.145% 之间。标准差为0.0737,T检验值为0.366,选取主要进口国含量不同的样品进行主含量的测定,与方法对比,其允差符合标准规定。应用本法日常检测,提具有高灵敏度和准确度,提高工作效率,用于大批量锰矿石的检测。     

Organic dust exposures from compost handling: case presentation and respiratory exposure assessment

This study was designed to determine the effects of age by decade on the efficacy of digital rectal examination (DRE) and serum prostate-specific antigen (PSA) for early detection of prostate cancer in men aged fifty and over. A prospective multicenter clinical trial was conducted at six university centers. All 6,630 male volunteers underwent a serum PSA (Hybritech, Tandem) determination and DRE. Quadrant biopsies of the prostate were performed if PSA was > 4 ng/mL or DRE suspicious. A total of 1,167 biopsies were performed, and 264 cancers were detected. The cancer detection rate increased from 3 percent in men aged fifty to fifty-nine to 14 percent in men eighty years or older (p < 0.0001). PSA detected significantly more of the total cancers than DRE at all age ranges (p < 0.05). The positive predictive values (PPV) for PSA were 32 percent (50-59 years), 30 percent (60-69 years), 34 percent (70-79 years), and 38 percent (80+ years). The corresponding PPVs for DRE were 17 percent, 21 percent, 25 percent, and 38 percent. Eighteen percent of the cancers were detected solely by DRE, whereas 45 percent of cancers were detected solely by PSA. Thus, the use of both tests in combination provided the highest rate of detection in all age groups. One hundred-sixty patients underwent radical prostatectomy and pathologic staging. Cancer was organ-confined in 74 percent (25/34) of men aged fifty to fifty-nine, 76 percent (65/86) of men aged sixty to sixty-nine, and 60 percent (24/40) of men aged seventy or over (chi 2, < 70 vs. > or = 70, p < 0.05). Early detection programs yield a lower, yet still substantial, cancer detection rate in younger men, and there is a greater likelihood for detection of organ-confined disease in this age range. Younger men have the longest projected life expectancy and, therefore, the most to gain from early prostate cancer detection.