扩散分离测定岩石中微量氯

于硫酸溶液中扩散分离氯,采用碳酸钠吸收,然后用硫氰酸汞—硫酸高铁铵比色法测定氯。本法重点研究了扩散分离富集微量氯的条件,共存离子对分离测定的影响。对严重产生干扰的溴碘离子,采用高锰酸钾氧化,8—羟基喹啉吸收办法消除。本方法氯最低检出限为0.71μg,标准偏差为13.19％。     

P-350萃取色层分离全差示分光光度法测定化探样品中痕量铀

样品制备为(1—2)mol/l HCl—2.5mol/l NaCl 介质,流经 P-350色层柱后,用0.5mol/l NaF 解脱色层柱上滞留的铀,衔接5-Br-PADAP,全差示分光光度法进行测定,方法的灵敏度在比色皿厚度b=3cm,微电流 i=6μA 时为0.00069μg/ml·0.01A′,相对标准偏差范围在3—19％。     

NUTRIENTS IN SEAWATER AND INTERSTITIAL WATER OF THE SEDIMENTS IN THE HUANGHE RIVER ESTUARINE AREA (NOVEMBER)

The investigation shows that the concentrations of nutrients are high in estuarine and coastal waters and low in offshore waters. The concentration of nitrate in estuaries is controlled through a physical mixing process and is also affected by hiotic activity. The annual transport of total inorganic nitrogen and dissolved phosphate-phosphorus from the Huanghe River water to the sea is about 8.45×104 and 1.45×103 tons respectively. The distributions of inorganic nitrogen and silicate in interstitial water of surface sediments are similar to those in surface and bottom sea water. Their contents in interstitial water are227 552μmol/l (average 375) for ammonia, 0.31 -9.0μmol/l (average 1.6) for nitrite, 0 41μmol/1 (average 6.0) for nitrate, and 41 139μmol/l (average 77) for silicate. The average concentrations of phosphate in the surveyed area are 0.64μmol/l for seawater and 1.2μmol/l for interstitial water. A cycle of phosphate in the estuary is also suggested in this paper.     

阴离子交换树脂分离—盐酸底液方波极谱法测定铜矿石中铅

利用铅离子在稀氢溴酸—溴化钾介质中能形成稳定络阴离子的特性,本文研究了应用717强碱性阴离子交换树脂分离大量铜等干扰元素、富集铅的最佳条件。试样经酸溶、预分离富集后,用方波极谱法在2mol/l HCl—1.25%VC 底液中测定铅。峰电位为-0.46V(对银片电极)。方法的检出限为0.98μg/g,测定限为1.96μg/g,相列标准偏差 R·S·D=8.7%,回收率在97%—110%之间。该方法分离干扰元素效果好,操作简便、快速,适用于铜矿石中2μg/g 以上铅的测定。也可用于岩石及其他矿物等复杂样品中微量铅的测定。     

污泥吸附剂制备的研究

为探索城市污泥资源化的途径,以城市污水处理厂的剩余污泥为原料,采用氯化锌活化法制备污泥吸附剂,考察了活化剂浓度、固液比、活化温度、活化时间4种因素对制备污泥吸附剂碘吸附值的影响,并对吸附剂进行了表征分析。实验结果表明:氯化锌浓度3mol/L、固液比1:2、活化温度550℃和活化时间40min为最佳制备条件,此条件下制得的污泥吸附剂碘吸附值为408.94mg/g,比表面积199.196m2/g,总孔体积为0.481cm3/g,微孔体积为0.089cm3/g,平均孔径为4.83nm。与商品活性炭相比,污泥吸附剂的碘吸附值和比表面积较小,孔径较宽,微孔所占比例较小,主要以过渡结构为主。     

全差示分光光度法测定地下水中微量酚

在PH10的碱性介质中,存在氧化剂铁氰化钾时,4-氨基安替比林与酚形成红色络合物,用三氯甲烷萃取比色测定酚,其检测限为0.002mg/l。但用二氯甲烷代替三氯甲烷萃取时,其检测下限可降低至0.0008mg/l。采用全差示分光光度法可进一步提高测定的灵敏度,其检测下限可降到0.00026mg/l。硫化物含量小于2.4mg/l时,对测定不干扰,可不预先蒸馏分离,而直接取样测定。     

含铜土壤中铜的物相分析

文章探讨了含铜土壤中铜的赋存状态 ,并对土壤中铜的物相分析方法进行了研究。结果表明 :用乙二胺浓度为 0 .0 5mol/L(pH =10 )的溶液浸取自由氧化铜 ,用含有Na2 SO3 和NH4 HF2 的H2 SO4 (0 .9mol/L)溶液浸取结合氧化铜 ,用含有硫脲 (2 0 0g/L)的HCl(1.0mol/L)溶液浸取次生硫化铜能获得满意的结果。在最佳浸取条件下对含铜土壤中的铜进行物相分析和基准矿物回收试验 ,结果满意。     

改性提高膨润土阳离子交换容量研究

研究了焙烧活化、酸活化、氯化钠活化、溴化十六烷基三甲铵活化等改性方法对膨润土阳离子交换容量的影响。结果表明,450℃焙烧2 h,膨润土阳离子交换容量可提高30%以上,0.01 mol.L-1氯化钠和0.3 mol.L-1溴化十六烷基三甲铵活化处理均可使膨润土阳离子交换容量提高10%以上,0.1 mol.L-1盐酸活化处理对提高膨润土的阳离子交换容量效果不明显,还深入讨论了改性提高澎润土阳离子交换容量的机理。     

三苯基膦泡沫塑料富集火焰原子吸收分光光度法测定微量银

试样经王水分解,在5％—15％的王水介质中,用三苯基膦泡沫塑料对微量银进行分离富集。用ρ为20g/l的硫脲溶液解脱被吸附在泡沫塑料上的银。解脱液在原子吸收分光光度计上测定银量。方法的检出限为0.022×10~(-■),特征浓度为0.014μg/ml,可测定地质样品中0.0X×10~(-6)以上的银量。     

海因类消毒剂对吉富罗非鱼的急性毒性

用溴氯海因(BCDMH)和二溴海因(DBDMH)两种消毒剂对吉富罗非鱼进行急性毒性试验,研究吉富罗非鱼对海因类消毒剂的耐受性。结果表明:溴氯海因对吉富罗非鱼苗的24 h LC50、48 h LC50和安全浓度分别为9.61、8.66、2.11 mg/L,二溴海因对吉富罗非鱼苗的24 h LC50、48 h LC50和安全浓度分别9.89、9.78、2.87 mg/L。     

Gas Bench Ⅱ-IRMS测定地下水中溴同位素新技术

建立了利用Gas BenchⅡ联用同位素比值质谱仪(Gas BenchⅡ-IRMS)用于测定地下水中溴稳定同位素的方法.基于溴比氯更容易被重铬酸钾氧化的性质,将Br-氧化成Br2,而氯残留在原溶液中,从而把溴与氯分离开;再利用AgNO3将溴以AgBr的形式沉淀下来,然后将AgBr转化成CH3Br进行溴稳定同位素质谱测定.反应中,CH3I用量为20 μL,AgBr用量为0.5 mg.本测试流程需溴4～10 mg,质谱测试时间由1.5h缩短为800 s,测试精度优于±0.1‰(2σ).该方法可以用于地下水中溴同位素测定,在水文地质研究中具有广阔的应用前景.     

Optimized one-step preparation of a bioactive natural product,guaiazulene-2,9-dione

We previously isolated a natural product, namely guaiazulene-2,9-dione showing strong antibacterial activity against Vibrio anguillarum, from a gorgonian Muriceides collaris collected in South China Sea. In this experiment, guaiazulene-2,9-dione was quantitatively synthesized with an optimized one-step bromine oxidation method using guaiazulene as the raw material. The key reaction condition including reaction time and temperature, drop rate of bromine, concentration of aqueous THF solution, respective molar ratio of guaiazulene to bromine and acetic acid, and concentration of guaiazulene in aqueous THF solution, were investigated individually at five levels each for optimization. Combined with the verification test to show the absolute yield of each optimization step, the final optimal condition was determined as: when a solution of 0.025 mmol m L-1 guaiazulene in 80% aqueous THF was treated with four volumes of bromine at a drop rate of 0.1 m L min-1 and four volumes of acetic acid at-5℃ for three hours, the yield of guaiazulene-2,9-dione was 23.72%. This was the first report concerning optimized one-step synthesis to provide a convenient method for the large preparation of guaiazulene-2,9-dione.     

Comparative study on the allergenicity of different Litopenaeus vannamei extract solutions

Allergen extracts are widely used for allergy diagnosis and treatment. The application of shrimp extract is hampered due to the low protein concentration and the inconsistent allergenicity. Extracting solutions are considered to be the primary limiting factor of protein extraction from crustaceans. This study aimed to select an optimal solution for shrimp protein extraction by comparing the allergenicity of different shrimp extracts. The effect of 7 existing or modified extracting solutions were evaluated, including the glycerol-NaCl solution, the glycerol Cocaine's solution, the buffered saline solution, the Cocaine's solution, the Glucose leaching solution, 1 mol L-1 KCl solution, and 0.01 mol L-1 phosphate buffered saline solution with and without dithiothreitolor(DTT). The quantitative(protein concentration) and qualitative parameters(SDS-PAGE protein patterns and immuno-reactivity) were determined using the sodium dodecyl sulfate polyacrylamide gel electrophoresis, enzyme linked immunosorbent assay and immunoblotting assay. Results showed that the 1 mol L-1 KCl solution with DTT was optimal for shrimp protein extraction, which yielded high concentration and allergenicity in the protein extract, including major and minor allergens. The 1 mol L-1 KCl solution with DDT is proposed for preparation of shrimp extract and associated allergy diagnosis, as well as potential applications for other crustaceans.     

D_（001）树脂在酸性硫脲溶液中吸附、分离金银研究

本文研究了Ｄ_００１大孔阳离子强酸树脂从Ｈ_２ＳＯ_４－ＣＳ（ＮＨ_２）_２溶液中，富集及分离Ａｕ（Ｉ）、Ａｇ（Ｉ）的性能。表明在ｐＨ＝２．０左右，树脂对Ａｕ（Ｔｕ）￣＋_２、Ａｇ（Ｔｕ）￣＋_２（Ｔｕ＝硫脲）有良好的吸附性能，Ａｕ和Ａｇ的吸附容量分别为６１．１８ｍｇ／ｇ－Ｒｅｓｉｎ和９９．１１ｍｇ／ｇ—Ｒｅｓｉｎ。负载柱上的Ａｕ、Ａｇ可分别用ＮａＣＮ—ＮａＯＨ和Ｈ_３ＢＯ_３－ＮａＯＨ－Ｎａ_２Ｓ_２Ｏ_３定量洗脱。可进行一定程度的Ａｕ、Ａｇ分离。     

水产饲料中三聚氰胺检测方法的优化

通过对高效液相色谱法(HPLC)测定水产饲料中三聚氰胺含量的方法进行优化,得到最佳色谱条件和前处理方法,建立了水产饲料中三聚氰胺的检测方法。结果表明:以体积比8∶92的乙腈、庚烷磺酸钠离子对试剂为流动相,柱温40℃,流速1.2 mL/min,以波长236 nm检测;以提取液为18 mL50%(φ)乙腈水+1 mL乙酸锌+1 mL1mol/L盐酸,淋洗液3 mL水和3 mL甲醇,洗脱体积6 mL作样品前处理。三聚氰胺加标回收率为85%～100%,相对标准偏差(RSD)小于5%,线性范围为0.2 mg/L～5.0mg/L,相关系数0.999 8,方法检出限为0.2 mg/kg。     

硼氢化钾还原——无色散原子荧光测定矿泉水及天然水中痕量硒

本文提出了一种新的测定矿泉水和天然水中痕量硒的测定方法。在严格控制加热温度的条件下,以硝酸-高氯酸为消解剂,在氢化物发生器中加入硼氢化钾水溶液后立即发生氢化反应,并生成 Se 元素的氢化物。在无极灯单色光下测定原子化后的 Se 元素激发的荧光强度。本方法灵敏、快速、可靠、操作方便。最低检出限为0.1ppb。     

磷锑钼蓝光度法测定红土镍矿中磷量

试样经烘干处理后,利用硫酸和氢氟酸溶矿,硝酸提取,加氨水以氢氧化铁为载体沉淀磷酸盐,分离镍、铬、钴、铜等干扰离子,制备成硝酸溶液。中和后,以钼酸铵—酒石酸锑钾为显色剂,以抗坏血酸为还原剂,显色,在700nm处测量吸光度,利用计算机拟合标准曲线计算磷含量。此方法精密度与加标回收率均能满足质量要求。     

COMPARATIVE STUDIES ON STRUCTURAL FEATURE OF AGAR POLYSACCHARIDES FROM PORPHYRA HAITANENSIS GROWN IN SOUTH AND NORTH CHINA

The structural feature of agar polysaccharides from Porphyra haitanensis grown in south China and transplanted to the north was investigated by fractioriation on DEAE - Sephadex A 50, chemical analysis, and infrared and 13C - NMR spectroscopy.The agars composed mainly of Charged molecules were eluted from DEAE - Sephadex A 50 with 1.0 mol/L- NaCl solution from the southern P. haitanensis and with 0.5 mol/L NaCl from the northern one. The 13C-NMR spectra showed that agarobiose [(1 -3)- B D - galactopyranosyl - (1 -4)-3,6-anhydro-a-L-galactopyranose] and the biological precursor of agarobiose [(1-3} B-D-galactopyra nosyl- (1-4)- 6- sulfate-a- L-galactopyranose ] were the major disaccharide repeating units in the charged fractions. The content of the biological precur sor in the agar polysaccharides from southern P. haitanensis was higher than that in the northern one, the content of the biological precursor extracted from cold water was higher than that from hot water, and the content of 6- OMe-D-galactos     

Simultaneous Determination of PIP and POP in Seawater

1INTRODUCTIONInrecentyearsglobalclimatechangehasbeenanissueofbothpublicandscientificconcern.Oceanscover71 %ofearthandplayamajorroleinglobalclimatechange.Phosphorus,asacriticalelement,regulatespri maryproductioninaquaticecosystems.Therefore,thefunctionofphosphorusinoceansystemhasreceivedin creasingscientificinterest(Songetal.,2 0 0 3 ) .PP (particulatephosphorus)isanimportantforminphosphorustransferinseawater(Song,2 0 0 1 ) .Pro portionofPPintotalphosphorus(TP)inseawatervar iesfrom 1 0 …