ANSI B74.

15-1992
(R2007)

ANSI B74.15-1992 (R2007)

Methods of
Chemical Analysis of Silicon Carbide
Abrasive Grain and Abrasive Crude

SPONSOR

Unified Abrasives Manufacturers Association

DEVELOPER

Grain Division
Approved April 30, 2007

ANSI
B74.15-1992
(R2007)

American National Standard

Methods of Chemical Analysis of Silicon

Carbide Abrasive Grain and Abrasive Crude

Approved April 30, 2007

American National Standards Institute, Inc.

American
National
Standard

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Published by

Unified Abrasives Manufacturers Association

30200 Detroit Road, Cleveland, Ohio 44145-1967

Copyright 2007 by Unified Abrasives Manufacturers Association

All rights reserved.
No part of this publication may be reproduced in any
form, in an electronic retrieval system or otherwise,
without prior written permission of the publisher.

Printed in the United States of America

ANSI B74.15-1992

Contents
Page
Foreword ........................................................................................................... iv
1

Scope............................................................................................................ 1

Reagents....................................................................................................... 1
2.1

General................................................................................................. 1

2.2

Concentrated acids and ammonium hydroxide .................................... 2

2.3

Diluted acids and ammonium hydroxide .............................................. 2

2.4

Ammonium chloride (NH4Cl)................................................................ 2

2.5

Ammonium oxaIate (NH4)2 C2O4 ....................................................... 2

2.6

Ammonium phosphate, dibasic (10%) ................................................. 2

2.7

Barium diphenylaminesulfonate (0.02%) ............................................. 2

2.8

Hydrogen peroxide solution (3% H2O2)............................................... 2

2.9

Hydrogen sulfide gas (H2S) ................................................................. 2

2.10 Hydroxylamine hydrochloride (10%) .................................................... 2

2.11 Lanthanum oxide.................................................................................. 2
2.12 Mercuric chloride (HgCL2) ................................................................... 2
2.13 Methyl red indicator solution (0.1%) .................................................... 2
2.14 Orthophenanthroline solution (0.1%).................................................... 2
2.15 Potassium chloride .............................................................................. 2
2.16 Potassium dichromate solution (0.01N) .............................................. 2
2.17 Potassium permanganate (0.01N) ...................................................... 2
2.18 Potassium permanganate (5%) ........................................................... 2
2.19 Potassium pyrosulfate (K2S2O7) ......................................................... 3
2.20 Ammonium acetate (30%) ................................................................... 3
2.21 Sodium carbonate, anhydrous (Na2CO3) ............................................ 3
2.22 Stannous chloride (5%) ....................................................................... 3
3

Filter papers .................................................................................................. 3

Preparation of samples of analysis ............................................................... 3

4.1

Abrasive crude ..................................................................................... 3

4.2

Abrasive grain ...................................................................................... 3

Blank determination ...................................................................................... 3

Page
Silicon Carbide Surface Analysis ................................................................... 3
6

Free silicon.................................................................................................... 3

Free silicon by hydrogen evolution ............................................................... 4

Free carbon (combustion)............................................................................. 5

Free carbon (induction) ................................................................................ 5

10 Loss on ignition ............................................................................................. 6

11 Free silicon and free silicon dioxide ............................................................. 6
12 Silicon carbide determined by potassium pyrosulfate fusion ........................ 8
13 Mixed oxides (R2O3 Group) ........................................................................... 8
14 Solution of mixed oxides ............................................................................... 9
15 Volumetric iron oxide determination.............................................................. 9
16 Colorimetric iron oxide determination ........................................................... 9
17 Colorimetric titanium dioxide determination ................................................ 10
18 Aluminum oxide .......................................................................................... 10
19 Calcium oxide determination....................................................................... 10
20 Magnesium oxide........................................................................................ 11
21 Analysis of the surface impurities of silicon carbide
by atomic absorption and colorimetry ......................................................... 11
21.1 Scope ................................................................................................. 11
21.2 Sample preparation ............................................................................ 11
21.2.1 Treatment procedure and solution sample A
for aluminum and iron analysis ............................................. 11
21.2.2 Solution sample B
for calcium and magnesium determination ........................... 11
21.3 Analysis of samples............................................................................ 11
21.3.1 Calibration standards................................................................. 11
21.3.2 Atomic absorption conditions for the analysis of samples ......... 12
21.4 Calculations........................................................................................ 12
21.4.1 Aluminum oxide ......................................................................... 12
21.4.2 Iron oxide ................................................................................... 12
21.4.3 Calcium oxide ........................................................................... 12
21.4.4 Magnesium oxide....................................................................... 12

ii

Page
21.5 CoIorimetric analysis of titanium dioxide ............................................ 12
21.5.1 Standards and calibration ......................................................... 12
21.5.2 Analysis of the sample .............................................................. 12
21.5.3 Calculation of titanium dioxide content ...................................... 12
Silicon Carbide Total Analysis ...................................................................... 13
22 Total carbonResistance furnace technique ............................................ 13
23 Total carbonInduction furnace technique................................................. 13
24 Silicon carbide determined by combustion ................................................. 13
25 Total silicon ................................................................................................ 13
26 Mixed oxides (R2O3 group).......................................................................... 14
Analysis of Powdered Silicon Carbide ......................................................... 14
27 Determine Fe, Al, Ti, Ca, Mg, as in sections 15 to 20 or 21 of
the silicon carbide surface analysis methods.............................................. 14
Definitions and Techniques ........................................................................... 14
28 Powdered silicon carbide analysis < 15m................................................. 14
29 Free carbon (combustion)........................................................................... 14
30 Free carbon (by induction) .......................................................................... 15
31 Free silicon dioxide ..................................................................................... 15
Figures
1

Combustion train carbon determination (resistance furnace) ....................... 6

Combustion train carbon determination (high-frequency

induction furnace) ......................................................................................... 7

iii

Foreword

(This Foreword is not part of American National Standard B74.15-1992)

The abrasive industry long recognized the need for the development of
uniform methods of chemical analysis for aluminum oxide abrasive grain
and abrasive crude. A committee within the industry was formed to develop
such standard methods. That committee completed its assignment in July of
1970, after approximately three years of concentrated effort. Final approval
as an ANSI document was received on May 5, 1971.
The document was reaffirmed without change in 1976. The Abrasive Grain
Association recognized that the standard would reflect substantial revision
in order to incorporate techniques which would reflect the current state of
the art. Therefore, the Chemical Procedures Sub-committee was formed in
1982 and given the task of reviewing and revising the standard. While the
committee worked on the revision and revising the standard. While the committee worked on the revision, the document was again reaffirmed without
change in 1983. Final revision was approved on January 9, 1986.
In 1991, the Analytical Procedures Subcommittee (formerly Chemical Procedures Subcommittee) reviewed and revised the document. Technical
Committee No. 2 on Loose Abrasives of ANSI B74 reviewed and approved
the revision. It was submitted for letter ballot to the ANSI B74 Standards
Committee on August 7, 1992. Final approval was received from ANSI on
December 23, 1992.
Standards are reviewed for reaffirmation or revision at least once in five
years. Suggestions for improvement which may be developed through the
use of this standard are welcome and should be sent to the Unified Abrasives Manufacturers Association, 30200 Detroit Road, Cleveland, Ohio
44145-1967.
The ANSI Accredited Standards Committee B74 on Abrasives, which reviewed and approved this standard had the following personnel at the time
of approval:
Roger Cloutier, Chairman
J. Jeffery Wherry, Secretary
Organization Represented
Name of Representative
Cemented Carbide Producers Association ................................. TBD
J. Jeffery Wherry (Alt.)
Exponent .................................................................................... Dr. Thomas H. Service
Compressed Air & Gas Institute.................................................. John H. Addington
General Services Administration ................................................ Steve Hooper
Industrial Diamond Association of America. Inc.......................... Ion Benea
Terry Kane (Alt.)
Society of Carbide and Tool Engineers....................................... Joseph B. Freiland
TechSolve ................................................................................... Anil Srivastava, Ph.D.
Unified Abrasives Manufacturers Association
Bonded Committee ................................................................... Roger Cloutier
Kevan Earl (Alt.)
J. Jeffery Wherry (Alt.)
Coated Committee .................................................................... John Hyde
Darrell DeGeus (Alt.)
Grain Committee....................................................................... Martin G. Wozniak
Phil Lockwood (Alt.)

iv

Organization Represented

Name of Representative

Superabrasives Committee....................................................... Mike Toke

Kevin Thomas (Alt.)

The personnel of Technical Committee No. 2 Loose Abrasives was as follows:

Martin G. Wozniak, Chairman
J. Jeffery Wherry, Secretary

Jerry Bandholz
Steve Hooper
Charles G. Hubbard
Phil Lockwood
Tom Martinez

Robert Mesanovic
Scott Pellow
Dave Rock
Frank Woodard