主题:C簇元素(C Si Ge Sn Pb)ICP分析手册

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tzl75
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主要包括一些元素的基本性质,标准储存及稳定性,样品的处理,谱线及干扰,检出现等内容,对新手很有指导作用.
Silicon

Location:  Group 14, Period 3
Atomic Weight:  28.0855
Coordination Number:  6
Chemical Form in Solution:  Si(OH)x(F)y2-


Storage & Handling:  Keep tightly sealed when not in use. Store and use at 20 ± 4°C. Do not pipet from container. Do not return portions removed for pipetting to container.

Chemical Compatibility:  Soluble in HCl, HF, H3PO4, H2SO4, and HNO3 as the Si(OH)x(F)y2-. Avoid neutral to basic media. Unstable at ppm levels with metals that would pull F- away (i.e. - do not mix with Alkaline or Rare Earths, or high levels of transition elements unless they are fluorinated). Stable with most inorganic anions with a tendency to hydrolyze forming silicic acid (silicic acid is soluble up to ~ 100 ppm in water) in all dilute acids except HF.

Stability:  2-100 ppb levels - stability unknown - (alone or mixed with all other metals) as the Si(OH)x(F)y2-. 1-10,000 ppm single element solutions as the Si(OH)x(F)y2- chemically stable for years in 2-5% HNO3 / trace HF in a LDPE container.

Si Containing Samples (Preparation & Solution):  Metal (soluble in 1:1:1 H2O / HF / HNO3); Oxide - SiO2, amorphic (dissolve by heating in 1:1:1 H2O / HF / HNO3); Oxide-quartz (fuse in Pt0 with Na2CO3); Geological Samples (fuse in Pt0 with Na2CO3 followed by HCl solution of the fuseate); Organic Matrices containing silicates and non volatile silicon compounds (dry ash at 450°C in Pt0 and dissolve by gently warming with 1:1:1 H2O / HF / H2SO4 or fuse / ash with Na2CO3 and dissolve fuseate with HCl / H2O); Silicone Oils - dimethyl silicones depolymerize to form volatile monomer units when heated (measure directly in alcoholic KOH / xylene mixture where sample is treated first with the KOH at 60 - 100°C to "unzip" the Si-O-Si polymeric structure or digest with conc. H2SO4 / H2O2 followed by cooling and dissolution of the dehydrated silica with HF). Note that the direct analysis of silicone oils in an organic solvent will result in false high results due to high vapor pressure of volatile monomer units such as hexamethylcyclotrisiloxane. The KOH forms the K2+Si(CH3)2O=NaCl, which is not volatile at room temperature.

Atomic Spectroscopic Information:  (red text indicates severe at ~ concs.)
Technique / Line Estimated D.L.* Order Type Interferences
ICP-OES 251.611 nm 0.012/.003 µg/mL 1 ion Ta, U, Zn, Th
ICP-OES 212.412 nm 0.02/.01 µg/mL 1 ion Hf, Os, Mo, Ta
ICP-OES 288.158 nm 0.03/.004 µg/mL 1 ion Ta, Ce, Cr, Cd, Th
ICP-MS 28 amu 4000 - 8000 ppt n/a M+ 14N2, 12C16O
*ICP-OES D.L.'s are given as radial / axial view



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Germanium
Location:  Group 14, Period 4
Atomic Weight:  72.59
Coordination Number:  6
Chemical Form in Solution:  Ge(OH)x(F)y2-


Storage & Handling:  Keep tightly sealed when not in use. Store and use at 20 ± 4°C. Do not pipet from container. Do not return portions removed for pipetting to container.

Chemical Compatibility:  Stable in HCl, HF, H3PO4, H2SO4, and HNO3 as the Ge(OH)x(F)y2-. Avoid neutral to basic media. Unstable at ppm levels with metals that would pull F- away (i.e. - Do not mix with Alkaline or Rare Earths or high levels of transition elements unless they are fluorinated). Stable with most inorganic anions with a tendency to hydrolyze.

Stability:  2-100 ppb levels - stability unknown alone or mixed with all other metals as the Ge(OH)x(F)y2-. 1-10,000 ppm single element solutions as the Ge(OH)x(F)y2- chemically stable for years in 2-5% HNO3 / trace HF in a LDPE container.

Ge Containing Samples (Preparation & Solution):  Metal (soluble in 1:1:1 H2O / HF / HNO3); Oxide - GeO (readily soluble in HCl or NaOH), GeO2 (fuse in Pt0with Na2CO3 followed by HCl solution of the fuseate); Geological Samples( fuse in Pt0 with Na2CO3 followed by HCl solution of the fuseate); Organic Matrices (dry ash at 450°C in Pt0 and dissolve by gently warming with 1:1:1 H2O / HF / H2SO4 or fuse ash with Na2CO3 and dissolve fuseate with HCl / H2O).

Atomic Spectroscopic Information:  (red text indicates severe at ~ concs.)
Technique / Line Estimated D.L.* Order Type Interferences
ICP-OES 164.919 nm 0.01/.001 µg/mL 1 ion Co, Fe, Cu
ICP-OES 219.871 nm 0.06/.009 µg/mL 1 atom W, Ir, Re, Co
ICP-OES 265.117 nm 0.05/.009 µg/mL 1 atom Ir, Re
ICP-MS 72 amu 20 ppt n/a M+ 36Ar2, 37Cl17O18O, 37Cl35Cl, 36S18O2, 36S2, 36Ar36S, 56Fe16O, 40Ar16O2, 40Ca16O2, 40Ar32S, 144Nd2+, 144Sm2+
*ICP-OES D.L.'s are given as radial / axial view


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Tin

Location:  Group 14, Period 5
Atomic Weight:  118.710
Coordination Number:  4, 5, 6, 7, 8
Chemical Form in Solution:  Sn(OH)xFy2-
(coordination numbers in green are observed less frequently)


Storage & Handling:  Keep tightly sealed when not in use. Store and use at 20 ± 4°C. Do not pipet from container. Do not return portions removed for pipetting to container.

Chemical Compatibility:  Soluble in HCl and dilute HF / HNO3. Avoid neutral to basic media. Unstable at ppm levels with metals that would pull F- away (i.e. - do not mix with Alkaline or Rare Earths or high levels of transition elements unless they are fluorinated). Stable with most inorganic anions, provided it is in the chemical form shown above.

Stability:  2-100 ppb levels stable (alone or mixed with all other metals that are at comparable levels) as the Sn(OH)xFy2- for 1 year in 1% HNO3 / LDPE container. 1-10,000 ppm single element solutions as the Sn(OH)xFy2- are chemically stable for years in 2-5% HNO3 / trace HF in a LDPE container.

Sn Containing Samples (Preparation & Solution):  Metal (soluble in HF / HNO3 or HCl); Oxides - SnO (soluble in HCl), SnO2 - very resistant to all acids including HF (fusion with equal parts of Na2CO3 and S is soluble in water or dilute acids as the thiostannate); Alloys (treat first 0.1 g with 10 mL conc. H2SO4 to boiling until the alloy disintegrates and nearly all of the sulfuric acid is expelled. Then add 100 mL O2 free water and 50 mL of conc HCl or transfer to a plastic container and add 1 mL HF, in either case, warming gently to bring about solution); Organic Matrices (volatility and precipitation of the insoluble stannic oxide are problems -- because these preparations are prone to error, we recommend you contact our technical staff at ivtech@ivstandards.com or (800) 569-6799 and we'll provide you with the necessary data for your specific sample type).

Atomic Spectroscopic Information:
Technique / Line Estimated D.L.* Order Type Interferences
ICP-OES 189.989 nm 0.03/.003 µg/mL 1 ion 
ICP-OES 242.949 nm 0.1/.01 µg/mL 1 atom W, Mo, Rh ,Ta, Co
ICP-MS 120 amu 5 ppt n/a M+ 120Te, 104Ru16O, 104Pd16O
*ICP-OES D.L.'s are given as radial / axial view


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Lead

Location:  Group 14, Period 6
Atomic Weight:  207.2
Coordination Number:  6
Chemical Form in Solution:  Pb(H2O)6+2


Storage & Handling:  Keep tightly sealed when not in use. Store and use at 20 ± 4°C. Do not pipet from container. Do not return portions removed for pipetting to container.

Chemical Compatibility:  Soluble in HCl, HF, and HNO3. Avoid H2SO4. Stable with most metals and inorganic anions forming insoluble carbonate, borate, sulfate, sulfite, sulfide, phosphate, oxalate, chromate, tannate, iodate, and cyanide in neutral aqueous media.

Stability:  2-100 ppb levels stable for months in 1% HNO3 / LDPE container. 1-10,000 ppm solutions chemically stable for years in 2-5% HNO3 / LDPE container.

Pb Containing Samples (Preparation & Solution):  Metal (best dissolved in 1:1 H2O / HNO3); Oxides (the many different Pb oxides are soluble in HNO3, with the exception of PbO2 which is soluble in HCl or HF); Ores and Alloys (best attacked using 1:1 H2O / HNO3); Organic Matrices (dry ash and dissolve in dilute HCl. Do not heat when dissolving to avoid precipitation of SiO2).

Atomic Spectroscopic Information:
Technique / Line Estimated D.L.* Order Type Interferences
ICP-OES 168.215 nm 0.03/.003 µg/mL 1 ion Co
ICP-OES 220.353 nm 0.04/.006 µg/mL 1 ion Bi, Nb
ICP-OES 217.000 nm 0.09/.03 µg/mL 1 atom W, Ir, Hf, Sb, Th
ICP-MS 208 amu 5 ppt n/a M+ 192Pt16O, 192Os16O
*ICP-OES D.L.'s are given as radial / axial view


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Carbon

Location:  Group 14, Period 2
Atomic Weight:  12.011
Coordination Number:  4
Chemical Form in Solution:  (Carbon standard is made using Tartaric Acid)


Storage & Handling:  Keep tightly sealed when not in use. Store and use at 20 ± 4°C. Do not pipet from container. Do not return portions removed for pipetting to container.

Chemical Compatibility:  Moderately soluble in HCl, HNO3, H2SO4, and HF aqueous matrices and very soluble in NH4OH. Stable with all metals and inorganic anions at low to moderate ppm levels. Do not dilute or store Carbon standards using plastic containers or similar devices.

Stability:  2-100 ppb level stability unknown. 1000-10,000 ppm level stable for years in dilute acidic media in a glass container.

C Containing Samples (Preparation & Solution):  elemental amorphic or graphitic carbon (Oxidative closed vessel fusion such as a Na2O2 fusion in a sealed Ni0 crucible / Parr bomb); H2CO3 (water soluble); Organic Compounds (water solubility is best if possible, or perform a Na2O2 fusion in a sealed Ni0 crucible / Parr bomb).

Atomic Spectroscopic Information:
Technique / Line Estimated D.L.* Order Type Interferences
ICP-OES 193.091 nm 0.05/.005 µg/mL 1 atom In, Ru, Mn
ICP-OES 247.856 nm 0.2/.02 µg/mL 1 atom Nb, V, Ti
ICP-MS 12 amu (uncertain) n/a M+ 
*ICP-OES D.L.'s are given as radial / axial view


zhy1005
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renzhihai
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tzl75
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whale
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原文由 zhy1005 发表:
拜托翻译一下


哈哈,这些都是专业方面的,大看一下应该能猜着的,
tzl75
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原文由 whale 发表:
C都可以用ICP测啊,太强了!



第一次听说吧,我算了算等离子发身光谱测定的不只是71个元素的
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