多波长法用于减小浊度对水源水中甲醛测定结果的影响

比较了减小水样浊度对样品结果影响的各种方法,包括过滤法、双波长法、三波长法,3种方法均基于乙酰丙酮分光光度法,测定波长均为414 nm。结果表明,以480 nm为参比波长的双波长法所得方法检出限为0.027 mg/L,采用470 nm与360 nm、460 nm与370 nm、450 nm与380 nm 3对参比波长的三波长法测得方法检出限为0.025~0.028 mg/L,这些方法用于检测0.100 mg/L标准点样品时,检测结果 RSD介于8.0%~8.6%。双波长法适合低浊度样品的直接分析,而浊度较高或双波长法测得结果大于方法检出限时,应采用三波长法进行定量分析,他们的使用有助于提高方法的准确度及减少工作量。用于地表水样品分析时,0.200、0.400 mg/L加标样品的回收率介于90.3%~101%,对应RSD介于0.0%~4.2%。     

多波长K系数方程法同时测定水样中的Cu~(2+)、Co~(2+)、Cd~(2+)

多波长Ｋ系数方程法同时测定水样中Ｃｕ２＋、Ｃｏ２＋、Ｃｄ２＋,即选定三个测定波长,分别将三组分在两个波长处的吸光度转换为另一波长处的吸光度,即可列出一个多元一次方程组,进而解出此波长处各组分的吸光度,求得各组分的含量。对水样中的Ｃｕ２＋、Ｃｏ２＋、Ｃｄ２＋三组分同时测定,结果令人满意。     

双波长K系数-紫外分光光度法同时测定水中硝酸盐氮和亚硝酸盐氮

基于吸光度的加合性原理,建立了双波长K系数—紫外分光光度法同时测定水中硝酸盐氮和亚硝酸盐氮的新方法。以水样中的两组分的峰值波长互为测定波长和参比波长,用解方程组法对两组分的吸光度分别进行解析,具有简便,快捷,灵敏度高的特点。方法适用于清洁水样或经处理的水样的分析,相对误差-2.7%～4.0%,相对标准偏差0.62%～5.09%,回收率92.3%～105.9%。     

校正吸光度的新方法

吸收光谱通常不是锐峰谱线,在待测组分的最佳定量波长处,其它组分即使有小量吸收,也干扰定量结果,在灵敏度较高的紫外分光光度法中尤为明显。色泽较深、浑浊或吸收光谱相互重迭的混合物,通常用双波长法校正吸光度能得到满意的结果。当散射光影响较大干扰杂质较复杂、干扰因素较多时,可以使用三波长法校正吸光度,这种新方法能更有效地消除干扰。     

总氮测定中的一点体会

在总氮测定中消解时间不够或高压锅压力不足 ,均会造成过硫酸钾分解不完全 ,从而导致空白吸光度偏高 ,标准曲线线性和结果重现性差。 ( 1 )样品消解 1 0、2 0、30、40 min,2 2 0 nm处的空白吸光度分别为 0 .378、0 .0 35、0 .0 1 5、0 .0 1 4,故样品至少需消解 30 min。 ( 2 )用家用高压锅消解样品 ,稍有漏气 ,消解 30 min,2 2 0 nm处的空白吸光度在0 .2 30～ 0 .874之间 ,空白吸光度高 (有时高于祥品吸光度 )且波动性大。不漏气情况下的空白吸光度在 0 .0 1 5左右 ,波动性小。因此消解时要注意观察高压锅是否漏气总氮测定中的一点体会@赵多…     

1-(2,6-二氯-4-硝基苯)-3-(4-硝基苯)-三氮烯光度法测定矿山废水中的锌

研究了用1-(2,6-二氯-4-硝基苯)-3-(4-硝基苯)-三氮烯(DCNPNPT)分光光度法快速直接测定锌的方法。在表面活性剂TritonX-15的存在下,pH=9.5～10.5的Na2B4O7-NaOH介质中,DCNPNPT与锌( )可生成1∶3的橙黄色络合物。最大吸收波长为445nm,同时在535nm配合物有一最大负吸收,建立以535nm为参比波长,445nm为测定波长的双峰双波长法进行测定,表观摩尔吸光系数可达1.12×105L/(mol·cm)。用拟定的方法测定矿山废水中的锌,与原子吸收法测定的结果十分吻合,结果令人满意。     

水中色度测定的研究

针对目视比色法色度测定不足之处,利用分光光度法进行改进.(1)在天然水的测定中,研究了以往的380nm作最大吸收波长测吸光度方法的问题.寻找到最佳波长455nm,吸收池5cm测定天然水吸光度A.(2)在5～400℃测定温度对吸光度无影响,溶液浊度、pH值对吸光度测定的影响呈线性关系.(3)在工业废水的测定中,先扫描出其最大吸收波长,以仪器检测限吸光度0.010为稀释终点.改进废水稀释倍数法.     

双波长分光光度法测定含硝酸盐水样中二甲基乙酰胺

紫外分光光度法是目前水中N,N-二甲基乙酰胺(DMAC)的常用分析方法。研究结果表明,硝酸盐对紫外分光光度法测定DMAC具有很强的干扰。本研究中提出一种双波长法用于消除水中硝酸盐的干扰作用,所采用的波长对为194.0nm和219.0nm。精密度实验及加标回收实验表明,方法的相对标准偏差在4%以内,回收率为95%~102%,可有效消除硝酸盐的干扰作用。     

原子吸收分光光度计用于冷原子吸收法测汞的试验研究

实验部分 一、原理及方法:汞蒸气对波长253.7nm的光有选择性吸收,在一定温度范围内,吸光度与汞蒸气浓度成正比。 水样经消化后,将各种形态的汞全部转化为二价汞离子,过量的氧化剂用盐酸羟胺还原,然后用氯化亚锡将汞离子还原为单质汞。在室温下,由载气将单质汞蒸气导入吸收管,在波长253.7nm处测定其吸光度,根据吸光度与浓度关系进行定量。用已知不同浓度的Hg离子标     

水体中总氮测定的影响因素及方法改进

对浊度、氯离子及高浓度氨氮对国标法测定总氮的影响进行分析。结果显示,浊度会使地表水中总氮测定的结果偏低,采用消解后3 500 r/min离心可以基本消除该影响;氯离子质量浓度3 000 mg/L时,对220 nm处吸光度值出现正干扰;水体中氨氮浓度较高时,会出现总氮测定结果严重偏低的现象,采用趁热摇匀法可以有效地避免高氨氮的干扰。     

Temporal-spatial variability and fractal characteristics of soil nitrogen and phosphorus in Xinji District, Hebei Province, China

Traditional statistics, geostatistics, fractal dimensions, and geographic information systems (GIS) were employed to study the temporal?Cspatial variability of soil total nitrogen (TN) and total phosphorus (TP) levels in Xinji District, Hebei Province area of the North China Plain from 1980 to 2007. The results indicate that nutrient levels follow normal or lognormal distributions. The TN content was 0.59 ±0.155 g kg^???1 in 2007, an increase of 0.44 g kg^???1 compared with that of 1980. In 2007, the TP content was 1.21 ±0.227 g kg^???1, an increase of 0.01 g kg^???1 from 1980. The geostatistical analysis showed that the distribution of these soil nutrients in the study area exhibits a trend and anisotropy. The range and [C ₀/(C ₀?+?C)] of TN and TP in 1980 were all less than in 2007. The ordinary kriging interpolation method was used to analyze the nutrient contents differences between 1980 and 2007. The results indicate that soil TN levels have increased over the 27-year period, and the area where the TN level had increased by at least 0.4 g kg^???1 was about 61.7% of the district. The area where the TP content increased covered about 58.4% of the district. The variance analysis indicated that land-use type had a clear influence on the distribution and change in TN and TP content. Using the 3-D box-counting dimension method combined with GIS, the fractal dimension of soil nutrient spatial distribution over the two periods showed that in 27 years, the fractal dimension of TN increased from 1.95 to 2.02, and the fractal dimension of TP increased from 1.89 to 2.01, indicating that the complexity of the spatial distribution of all nutrient contents had increased. This study can provide a basis for accurate fertilizing and to enhance the conversion of soil characteristics under different spatial scales.     

一种便携式荧光测油仪在海上溢油应急监测中的适用性研究

研究了一种便携式荧光测油仪在海上溢油应急监测中的适用性,并与现行仲裁标准方法进行比较分析。研究表明:该便携式荧光测油仪测定海水中油类样品仅需100 mL水样,平均每个样品所需的前处理时间约340 s,方法检出限为0.003 mg/L,测定下限为0.012 mg/L。测定用标准物质配制的不同浓度海水样品,相对标准偏差为0.08%~0.87%,测定标准样品的相对误差为0.49%~4.50%,实际样品加标回收率为90%~107%。对标准物质配制的海水样品进行检测,与现行仲裁标准方法在0.05水平下无显著性差异。在渤海中部海上监测中,连续6 d测定不同标准样品的相对标准偏差为0.26%~0.83%。研究结果表明,该便携式荧光测油仪适用于现场对油类的定量分析和水质评价。     

纳氏试剂法检测水中低浓度氨氮存在问题分析及方法改进探讨

针对采用《水质氨氮的测定纳氏试剂分光光度法》(HJ 535—2009)测定低浓度氨氮时存在的测不准问题,研究了药剂投加量、反应时间等因素对检测结果的影响,认为低浓度氨氮下的显色反应速度过慢是测定结果不准的原因,并据此提出利用强碱调节pH的方法加速反应进程。改良后的方法可以在0.2～1.2 mg/L氨氮浓度范围内呈现良好的线性关系,相关系数r为0.999 4。该方法具有较高的准确度和精密度,有效扩大了低浓度氨氮的检测范围,在实际样品检测中的回收率为102.5%～115.0%,可为准确测定水环境和饮用水中的氨氮浓度提供一种简便易行的手段。     

Evaluation of optimal conditions for determination of low selenium content in shellfish samples collected at Todos os Santos Bay,Bahia, Brazil using HG-AFS

This work proposes a procedure for the determination of total selenium content in shellfish after digestion of samples in block using cold finger system and detection using atomic fluorescent spectrometry coupled hydride generation (HG AFS). The optimal conditions for HG such as effect and volume of prereduction KBr 10 % (m/v) (1.0 and 2.0 ml) and concentration of hydrochloric acid (3.0 and 6.0 mol L^?1) were evaluated. The best results were obtained using 3 mL of HCl (6 mol L^?1) and 1 mL of KBr 10 % (m/v), followed by 30 min of prereduction for the volume of 1 mL of the digested sample. The precision and accuracy were assessed by the analysis of the Certified Reference Material NIST 1566b. Under the optimized conditions, the detection and quantification limits were 6.06 and 21.21 μg kg^?1, respectively. The developed method was applied to samples of shellfish (oysters, clams, and mussels) collected at Todos os Santos Bay, Bahia, Brazil. Selenium concentrations ranged from 0.23?±?0.02 to 3.70?±?0.27 mg kg^?1 for Mytella guyanensis and Anomalocardia brasiliana, respectively. The developed method proved to be accurate, precise, cheap, fast, and could be used for monitoring Se in shellfish samples.     

ICP-AES法多条谱线测定环境土壤中钒

选用钒的5条特征谱线用电感耦合-等离子发射光谱(ICP-AES)法测定环境土壤中的钒含量,运用干扰系数法对多个土壤标样和样品测定结果进行干扰校正,干扰系数用多个土壤标样的标准值和测定值的最小二乘法来确定.结果表明,未进行校正时,7个土壤标样5条特征谱线测定原始结果和标准值相差较大,不在标准值的范围内；校正后,土壤标样的311.071 nm.波长与309.311 nm波长谱线测定结果的均值在范围之内,且干扰系数为1.015(约等于1),不需折算,波长311.071 nm也在保证值范围内(校正系数为1.184).对土壤样品进行测定,5条谱线测试结果一致性好,相对标准偏差为2.2％～10.4％,平行相对偏差为0.3％～3.3％,加标回收率为88.4％ ～ 111.4％.建议用ICP-AES法对环境土壤中的钒测定时,选用波长311.071 nm谱线并用干扰系数法进行校正(系数为1.184),或用波长311.071 nm与309.311 nm谱线测定均值作为测定结果.     

Planted floating bed performance in treatment of eutrophic river water

The objective of the study was to treat eutrophic river water using floating beds and to identify ideal plant species for design of floating beds. Four parallel pilot-scale units were established and vegetated with Canna indica (U1), Accords calamus (U2), Cyperus alternifolius (U3), and Vetiveria zizanioides (U4), respectively, to treat eutrophic river water. The floating bed was made of polyethylene foam, and plants were vegetated on it. Results suggest that the floating bed is a viable alternative for treating eutrophic river water, especially for inhibiting algae growth. When the influent chemical oxygen demand (COD) varied from 6.53 to 18.45 mg/L, total nitrogen (TN) from 6.82 to 12.25 mg/L, total phosphorus (TP) from 0.65 to 1.64 mg/L, and Chla from 6.22 to 66.46 g/m³, the removal of COD, TN, TP, and Chla was 15.3 %–38.4 %, 25.4 %–48.4 %, 16.1 %–42.1 %, and 29.9 %–88.1 %, respectively. Ranked by removal performance, U1 was best, followed by U2, U3, and U4. In the floating bed, more than 60 % TN and TP were removed by sedimentation; plant uptake was quantitatively of low importance with an average removal of 20.2 % of TN and 29.4 % of TP removed. The loss of TN (TP) was of the least importance. Compared with the other three, U1 exhibited better dissolved oxygen (DO) gradient distributions, higher DO levels, higher hydraulic efficiency, and a higher percentage of nutrient removal attributable to plant uptake; in addition, plant development and the volume of nutrient storage in the C. indica tissues outperformed the other three species. C. indica thus could be selected when designing floating beds for the Three Gorges Reservoir region of P. R. China.     

Quantitative detection of nitrate in water and wastewater by surface-enhanced Raman spectroscopy

The presence of inorganic nitrogen species in water can be unsuitable for drinking and detrimental to the environment. In this study, a surface-enhanced Raman spectroscopy (SERS) method coupled with a commercially available gold nanosubstrate (a gold-coated silicon material) was evaluated for the detection of nitrate and nitrite in water and wastewater. Applications of SERS coupled with gold nanosubstrates resulted in an enhancement of Raman signals by a factor of ～10⁴ compared to that from Raman spectroscopy. The new method was able to detect nitrate with linear ranges of 1–10,000 mg NO₃ ^?/L (R ²?=?0.978) and 1–100 mg NO₃ ^?/L (R ²?=?0.919) for water and wastewater samples, respectively. Among the common anions, phosphate appeared to be the major interfering anion affecting nitrate measurement. Nevertheless, the percentage error of nitrate measurement in wastewater by the proposed SERS method was comparable to that by ion chromatography. The nitrate detection limits in water and wastewater samples were about 0.5 mg/L. The SERS method could simultaneously detect sulfate, which may serve as a reference standard in water. These results suggested that the SERS coupled with nanosubstrates is a promising method to determine nitrate concentrations in water and wastewater.     

一氧化氮标准气体中二氧化氮杂质FTIR定量方法研究及标气质量分析

一氧化氮标准气体在我国空气质量监测工作中广泛用于氮氧化物分析仪的校准,标准气体的质量对环境空气中氮氧化物的测量结果也有着显著的影响.利用傅里叶变换红外光谱仪建立了一套精确测量低浓度二氧化氮方法,并对一氧化氮标准气体产品中二氧化氮杂质进行了测量.结果显示有少部分样品中存在较高浓度的二氧化氮杂质.进一步讨论了可能导致一氧化...