Precision and accuracy in trace element analysis of geological materials using solid source spark mass spectrography

Nicholls, G. D.; Graham, A. L.; Williams, E.; Wood, Mary McGee

doi:10.1021/ac60250a018

Cited by 102 publications

(33 citation statements)

References 17 publications

(1 reference statement)

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“…The ionization efficiency of the spark is dependent upon the sample matrix (34). Good standard samples with matrices similar to that of the ash are needed to calculate accurate relative sensitivity coefficients for the elements (35). The ash contains most of the elements in the earth's crust which results in a very complex rrass spectrum.…”

Section: Figure I~l Periodic Tablementioning

confidence: 99%

“…Care must be taken not only to insure the homogeneity of the sample and sample-graphite mixture, but also the homogeneity of the internal standard in the electrodes if the doping method is used (172,178). Homogenizing methods vary from simple grinding and thorough mixing to complex methods of dilution by multiple fusion (35,188). The error due to sample electrode inhomogeneity can be less than 5% (35,36,174).…”

Section: Photographic Detectionmentioning

confidence: 99%

“…Homogenizing methods vary from simple grinding and thorough mixing to complex methods of dilution by multiple fusion (35,188). The error due to sample electrode inhomogeneity can be less than 5% (35,36,174). The shape of the sample electrodes should be consistent (28,38,179,180).…”

Section: Photographic Detectionmentioning

confidence: 99%

“…The shape of the sample electrodes should be consistent (28,38,179,180). The spark parameters (e_.£., repetition rate, pulse length) and spark gap width should be constant (28,35,38,171,173,178,177,(179)(180)(181)(182)(183). These parameters affect the relative elemental ionization efficiency in the spark and the ion charge distribution in the spark plasma (31, 173,178,183).…”

Section: Photographic Detectionmentioning

confidence: 99%

“…The accuracy of the determination of the relative sensitivity of this method for elements in a certain sample matrix affects the precision and accuracy of the analysis (28,31,(34)(35)38,(171)(172)(173)(174)(175)(176)(177)(178)(180)(181)(182)185,(188)(189)(190)(192)(193)(194)(195)(196). The relative elemental sensitivity is dependent on the elemental ionization potential (36,38,172,175,176,180,185,189,192), volatility (35,36,38,172,175,176,180,182,185,189,192), and ionization cross-section, which is determined by the atomic covalent radius (172,175,…”

Section: Photographic Detectionmentioning

confidence: 99%

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Section: Figure I~l Periodic Tablementioning

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Section: Photographic Detectionmentioning

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Improvement in the analysis of ashes from coal by spark source mass spectrography

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Quantitative Spark Source Mass Spectrometry

Morrison

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knowledge of t h e chemical c o m p o s i t i o n of m i n e r a l s , a l l o y s , r e s i d u e s and h i g h p u r i t y m a t e r i a l s . Spark s o u r c e mass s p e c t r o m e t r y (SSMS) i s p l a y i n g a n e v e r i n c r e a s i n g r o l e i n t h e f i e l d of m a t e r i a l s c h a r a c t e r i z a t i o n by t r a c e m u l t i e l ement a n a l y s i s . IJnder i d e a l c o n d i t i o n s SSMS c a n b e used t o a n a l y z e for a l l s t a b l e e l e m e n t s a t l e v e l s r a n g i n g from a l m o s t 1% t o a few p a r t s p e r b i l l i o n .Normally no p r e c o n c e n t r a t i o n i s r e q u i r e d and sample p r e t r e a t m e n t i s m i n i m a l . Furthermore, SSMS d o e s n o t e x h i b i t order-of-magnitude v a r i a t i o n s i n s e n s i t i -v i t y for d i f f e r e n t e l e m e n t s i n a g i v e n matrix as do n e u t r o n a c t i v a t i o n a n a l ys i s and atomic a b s o r p t i o n s p e c t r o s c o p y . However, SSMS has s u f f e r e d from a r ep u t a t i o n of b e i n g o n l y a s e m i q u a n t i t a t i v e t e c h n i q u e b e c a u s e o f t h e d i f f i c u l t y i n v o l v e d i n p r o p e r l y c a l i b r a t i n g t h e a n a l y t i c a l d a t a o b t a i n e d . C o n t r i b u t i n g t o t h e problem h a s been t h e slow r e c o g n i t i o n a n d s u b s e q u e n t e l i m i n a t i o n of v a r i o u s s y s t e m a t i c e r r o r s a f f e c t i n g t h e a n a l y s i s .A s e m i q u a n t i t a t i v e e s t i m a t e of t r a c e element c o n c e n t r a t i o n can b e made from a v i s u a l comparison o f e x p o s u r e s n e c e s s a r y t o produce j u s t d e t e c t a b l e l i n e s from a t r a c e element i s o t o p e and a n i s o t o p e o f a r e f e r e n c e element.Trace element c o n c e n t r a t i o n s c a n t h e n b e c a l c u l a t e d from t h e f o l l o w i n g equa-where t h e s u b s c r i p t s s and i r e p r e s e n t t h e i n t e r n a l s t a n d a r d and t r a c e e l e m e n t r e s p e c t i v e l y , C -c o n c e n t r a t i o n i n ppm(wt.1, X -c o n c e n t r a t i o n o f i n t e r n a l s t a nd a r d , Ezbeam m o n i t o r e x p o s u r e i n coulombs o f c h a r g e f o r e q u i v a l e n t peak i nt e n s i t i e s of t h e t r a c e element and s t a n d a r d s p e c i e s ( j u s t d e t e c t a b l e l i n e s

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The Determination of the Rare Earth Elements in Rocks by Spark Source Mass Spectrometry

Puymbroeck

Gijbels

1978

Bulletin des Soc Chimique

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ABsmAcTThe determjnation of the rare earth elenents i n rocks by high frequency spark source nass spectmmetry, using photoplate detection, was investigated.Several standard m c k s (ECR-1, JE-1, JG-1, W-G, NIM-N) were analysed by the "direct" method, and after thre different selected e n r i c h t prcedures: peroxide fusion and succc?ssive hydroxide and fluoride precipitations; acid digestion and cation exchange chrcmatography; acid digestion and mixed-solvent anion exchange chranatqraphy. These premncentration methods are discussed and the results o b W are canpared w i t h each other.A mixed-solvent anion em3mngmpcedm-e permits t o & d n e rare earth e l m t s w i t h a precision of 10 %.The concentration of the rare earth elewnts (E) i n rccks can be determiner? by several awlytical techniques. Neutron activation analysis (NAA) is most widely used. other m esuch a s X-ray fluorescence (xI7F) and mass q e c t r a m t r i c isotope dilution (InG) are also ccnonly employed. A pranising and frequently used technique is high frequency spark source mass spectrcmetq (SSMS) or lowvoltage discharge mvce mass -.For the determination of the lanthanides scme of these methcds can be used without any Fellminary sample treatmnt (instnnwtal NAA) , or with a very s-le pretreatment (SSMS).The other tedpiques need a premruzntration or separation step of the REE (m, radicchmical tw&, )(RF). when dealing w i t h amunts i n the ultra trace region ( < 1 ppn), concentration a d -ation steps must, i n practice, be introduced regardless the technique used.In this rrork, the applicability of high frequency spark source mass spxtrcpnetry, using photoplate detection, was investigated.A t f i r s t , the rock p d e r and the graphite were mixed directly with each other and sparked. (1-9). "his method could not yield very accurate results for a l l rare earth e l m t s and its Rensitivity was insufficient i n the u l t r a trace region.In order to eliminate interferences f m major elements and to be able to determine mre accurately a l l REE, even i n the ultra trace region, three different concentration and separation p -s were investigated:

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Precision and accuracy in trace element analysis of geological materials using solid source spark mass spectrography

Cited by 102 publications

References 17 publications

Improvement in the analysis of ashes from coal by spark source mass spectrography

Improvement in the analysis of ashes from coal by spark source mass spectrography

Quantitative Spark Source Mass Spectrometry

The Determination of the Rare Earth Elements in Rocks by Spark Source Mass Spectrometry

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