Astm stp 542 1973

THE ANALYSIS OF SLAGS AND RELATED OXIDE TYPE MATERIALS () Á symposium presented at the PiHsburgh Conference Cleveland, Ohio, Z7 March 1973 sponsored by ASTM E 2 on Emission Špectroscopy ASTM SPECIAL T[.]

Contents

Introductory Remarks G L Mason

The Application of Multi-Channel Spectrometers to the

Elemental Analysis of Oxide Materials W Ramsden,

Applied Research Laboratories, Ltd., Luton (Beds.),

England

Current Status of X-Ray Emission Analysis for the Analysis

of Slags and Related Oxide-Type Materials -R Jen-

kins, Philips Electronic Instruments, Mount Vernon,

N, Y 10550

Atomic Absorption Spectrophotometry in the Analysis of Slags

and Oxides M D A m o s , Varian Techtron Pty Ltd.,

Melbourne, Australia 3171

Utility of the Optical Emission Spectrometer in the Analysis

of Refractories, Slags, and Other Oxide Materials

J R Ryan and R K Scott, Garber Research Center,

Harbison-Walker Refractories, Division of Dresser In-

dustries, Inc., Pittsburgh, Pa 15227

X-Ray Emission Spectrometer Analysis of Slags and Related

Materials J C Cline and R A Pontello, Globe

Metallurgical Corp., Division of Interlake, Inc., Bev-

erly, Ohio 45715

Analysis of Slags by Atomic Absorption Spectrophotometry

H G Zelinske and D H Arendt, Amsted Research

Labs., Bensenviile, Ill 60106

Questions and Answers

1 con- tinued Side 2

STP542-EB/Mar 1973

W Ramsden

The Application of Multi-Channel

Spectrometers to the Elemental

Analysis of Oxide Materials

2 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

Fig 2 Effect O f Grind;ng Time on XRF Analysis Of Sinters

RAMSDEN ON MULTI-CHANNEL SPECTROMETERS 3

4 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

RAMSDEN ON MULTI-CHANNEL SPECTROMETERS 5

1000 2000 m volts

6 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

12 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

TABLE 1

COMPOSITION OF INDUSTRIALLY IMPORTANT OXIDES

Iron Ore Fe Refractories Cement

Constituent ~ S~gs Ceramics Limestone Glass

0.02 0.05-0.5 0.01-11 0.1-3 0.5-1.5 0.06-3 1-55 10-15 0.01-2 0.1-0.2

3-6

0.5-3

0.5-50

,,DAY-TO-DAY REPRODUCIBILITY OF IRON ORE SINTER ANALYSIS

"" - ( QUA NTOVA~:" - I~R'IQUETTE )-"

Day Fe CaO $ 1 0 2 P 2 0 5 MnO MgO AI203 S

RAMSDEN ON MULTI-CHANNEL SPECTROMETERS 13

TABLE 3

PERFORMANCE OF MULTICHANNEL XRF SYSTEMS

ON OXIDE MATERIALS ( i960-65 )

Prec ~slan Accuracy

Material Constituent s.cl at %o A ~ / O Range

AFTER F U S I O N - I R O N ORE SINTER ( 1 : 5 ) Grinding Hme (mln) 0.5 4

14 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

Na K~ 11.909 A 4" RAP Flow Prop P-10 P.H.D

Mg Kin 9.889~, 4" ADP Ne Prop AI Window P.H.D

AI K~ 8.339 ~ 4"E DDT Ne Prop AI Window P.H.D

Si K~ 7.126 ~ 4"E DDT Ne Prop Be Window P.H.D

P Ke, 6.155 ~ 4" Ge Ne Prop Be Window P.H.D

S K~ 5.373 ~ 4" Ge Ne Prop Be Window P.H.D

K Kel, 3.744 ~ 4" LiF Ne Multltron Be Window

Ca K4 3.360 ,~ 4" LiF Ne Multitron Be Window

Ti Ke 2.750 ~ 4" LIF Ne MulHtron Be W~ndow

Cr Kdl 2.291 ~ 4" LiF Ne Multitron Be Window

Mn K6 2 103 ~ 4" LiF Ne Multltron Be Window

Fe Kei 1.937 ~ 4" LIF Ne Multitron Be Window

X-ray Tube: Rh; 50 Kv 40 ma

TA B LE 7 COMPARISON OF SHORT-TERM PRECISION OF

72000 - FUSION TECHNIQUE ( 1972 ) AND

( < 0.05%)

Systematic errors

I Sampling

I Sample Absorption 1100%1 errors Enhancement (10%)

Particle effects (100%) Chemical state (5%) Equipment errors ( <~ 0.05%) Note: All errors quoted are given in terms of 1 O"

Figure ~1

16 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

Phase Fluorescing element Absorption for Effect

factor pj(x)

C(~.~j)= ~i ci [ F i ( J L ) + A ' ~ i ( ~ ' J ) 1

JENKINS ON CURRENT STATUS OF X-RAY EMISSION 17

18 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

11

9 crystal s p e c t r o m t e r J j

Wawlan~)th~

Comparative resolutions of the flow counter, the scintillation counter, the semiconductor

counter, end the crystal spectrometer

Figure # 6

FIG 1 Concentration of Analyte = 0-100 ~o Solution of l g / 1000 ml

Dilution is 1000:1 Concentration in Solution is 1.00 mg/I

If Analytical Measurement is in Error by 1~o ( + v e )

Concentration Found will be 1-01 m g / I and Result Obtained will be 0.101 ~ i.e 1 ~o Error

2 0 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

F I G 5

DISADVANTAGES OF SOLUTION METHODS

1 Requirement to Devise Solution Method

2 Additional Handling

3 Possibility of Dilution

or Calculation Errors

F I G 6

ADVANTAGES OF SOLUTION METHODS

1 Minimization of Inhomogeneity Errors

2 Ideal "lso Formation"

AMOS ON ATOMIC ABSORPTION SPECTROPHOTOMETRY 21

FIG 11

Concentration Ranges (%) ( 1 g / 100 ml )

Detection Limit 0.00001 0.00005 0-0002 0.0025 0.0002 Abs = 0 8 8 0.02 0.125 1.5 3 0.06 Burner at 90 ~ 0-4 2-5 30 60 1.2

F I G 12

STP542-EB/Mar 1973

] R Ryan and R K Scott

Utility of the Optical Emission Spectrometer

in the Analysis of Refractories, Slags, and Other Oxide Materials

N o Figures or Tables

STP542-EB/Mar 1973

J C Cline and R A Pontello

X-Ray Emission Spectrometer Analysis of

Slags and Related Materials

F I G 1

24 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

TABLE i CR2~ "SWEDE SLABS

NO, C ERTIFIED DIRECT ~USION R ~ '

ADJ, COEF OF COREL 9973 ,9991

STIr, ERROR OF EST, ,0741 ,0442

$TI) ERROR OF EST 1.4098 4321 4883

TABLE 3 FEO "SWEDE SLAGS

$TI), ERROR OF EST, !,40BO I,ii08 ,g137

CLINE AND PONTELLO ON X-RAY EMISSION SPECTROMETER 25

TABLE AL203 *SWEDE SLAGS

HV, ABS, CERTIFIED DIRECT FUSIO~ FUSION

26 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

TABLE 3A FEO (R'FE = P~E EXP S PC.A) Z

PJSICCI II.A Ft:SIO(I

tl~ CERTIFIEI) O~ SF_RVD Ca~CTED OP3FJT.~EI) COR~_CIT~

STP542-EB/Mar 1973

H G Zelinske and D H Arendt

Analysis of Slags by Atomic Absorption

Spectrophotometry

PERCENT CONCENTRATION HAN4Jrs OF SLAG CONSTITUENTS CONSTITUENT % CONC RANGE SILICON OXIDE 0 - 8 0 0 CALCIUM OXIO( 0 m 8 0 0 ALUMINUM OXIDE 0 - - DO.O IRON OXIOE 0 - - 5 0 0 CHROMIUM OXIDE 0 - - 4 8 , 0 MAGNESIUM OXIDE O - - 4 O O MANGANESE OXIDE 0 - 3 0 0 TITANIUM OXIDE O - - I Z6

28 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

ZELINSKE AND ARENDT ON ANALYSIS OF SLAG 29

30 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

ZELINSKE A N D ARENDT ON ANALYSIS OF SLAG 31

32 ANALYSIS OF SLAGS AND RELATED OXIDE-TYPE MATERIALS

SILICON OXIOE 4 5 6 0 4 5 5

FIG 12

BASIC SLAG B.C.S NO 174 1 CONSTITUENT

LAB A LAB, S AMSTED