Production of Low Cost Spectrometer Drift Correct Standards

By: Phillip Kubichka, Advisor: Kyle Metzloff

A water cooled mold and the required core boxes to create spectrometer drift correct standards were
produced at the University of Wisconsin-Platteville. Although multiple heats have occurred, samples fit
for use as spectrometer standardizing material have yet to be produced. However, the work completed
thus far has been vital in proving designs and concepts for the creation of samples. The techniques and
processes require further refinement in key areas of core binder selection and possible iron treatment to
become fully feasible.

Objectives

To develop and refine a method for producing chill cast spectrometer drift correct standards on a small

scale of 50+ samples per heat in the UW-Platteville foundry.

Introduction

Production of white iron standards on a large scale of 500+ samples per pour has been studied

previously. Multiple parties have expressed interest in a production technique capable of producing

small batch size heats allowing them to produce samples of customized chemistries.

Terminology

Pour A single event of a mold being filled with iron. Multiple pours may take place from a heat.

Heat A single amount molten metal in the furnace, all with the same base chemistry that may be

poured over multiple molds. Multiple pours can take place from a single heat.

Types of Reference Material

RM - Reference Material

Material whose property values are sufficiently homogeneous and well established to be used for

calibration of an apparatus

CRM - Certified Reference Material

Reference material accompanied by a certificate indicating that chemical values are tested by an

accurate and traceable method including uncertainty values

SRM Standard Reference Material

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Certified Reference material that also meets additional NIST-specific certification criteria and is issued

with a certificate of analysis that provides information regarding its appropriate use.

History and Past Research into Producing Reference Material

The National Bureau of Standards, currently known as the National Institute for Standards and

Technology (NIST) produced the publication 260-1 titled Preparation of NBS White Iron

Spectrochemical Standards in 1964. This document details the production process, techniques and

materials needed for producing a large scale mold of 500+ samples per pour.

The Metals Research and Development Foundation produced project 169, titled Spectrometric

Standards in 1983 to fill chemistry vacancies of the original NIST standards of 1964. This report details

changes to sample shape and marking techniques from the 1964 NBS publication.

The Iron Casting Research Institute (ICRI) lead an investigation into the production methods for

spectrographic samples. The investigation was spearheaded by Pete Meyst and included process

observations from ACIPCO foundry. A document titled Tentative CRM Production Method was

produced in 2002 and instructed exactly what was needed for a large scale production, 500+ samples per

pour, and techniques behind successful pours.

Individual Foundries provided personal experience, tips and techniques for their current trials for scaling

down the process to a small scale production of spectrometer standards. These foundries include

Waupaca Foundry, Neenah Foundry, and Grede Foundry.

Production of Spectrometer Standards at UW-Platteville

Production methods, materials, and procedures shall be constructed, drafted, verified and published for

creation of reference material suitable for calibration of an emission spectrometer. This includes

creation of a water cooled mold along with all necessary working core-boxes.

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Knowledge of this research is to be made publicly available through the American Foundry Society and

to any interested parties.

Apparatus

Solidcast Software Palmer Vibrating Molding Bench

Magma Software Induction Power Supply
Mastercam Software Tilt Pour Iron Furnace
4 Axis Milltronics Vertical Mill Ductile Iron Treatment Vessel
2 Axis Milltronics Vertical Mill Ladle Preheating Torch
Water Cooled Copper Mold Electro-Nite Datacast 2000
Miller Shopmaster Welder Pyrometer
Palmer Continuous Mixer

Figure 1 Water Cooled Copper Mold Figure 3 2 Axis Milltronics Vertical CNC Mill

Figure 4 Palmer M50XL Continuous Mixer and

Figure 2 4 Axis Milltronics Vertical CNC Mill
Palmer Vibrating Molding Bench

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Figure 5 Pillar MK8 100kw 3000HZ Induction
Power Supply
Figure 8 Electro-Nite Quik-Lab Datacast 2000

Figure 6 Tilt Pour Iron Furnace 135lb

Capacity, Ductile Iron Treatment Vessel, and
Belch Fire Lade Preheat Torch

Figure 9 Miller Shopmaster 300 AC-DC Welder

Figure 7 Hand Held Pyrometer and Extra

Thermocouple Tips Sitting Atop the Furnace
Cooling Pump

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Procedure

Sample Design

General sample size and shape must first be determined with the following conditions in mind

Figure 10

a) How will the sample be ground, by hand or mechanically?

b) What is the expected chill depth?

c) Will a specific shape produce a uniform structure?

A plate arrangement of samples and sample spacing is then determined with the following

conditions in mind Figure 11

Realistic sand core thickness between samples

d) Minimum sample separation distance for minimal side heat flow

e) Maximum mold size via machine and budget limitations

Gating Design

1) A pressurized gating system design is created following standard gating principals and

having the following criteria in mind

a) Minimal heat flow from gating system to the samples

b) Fast and complete mold filling Table 4

c) Easy sample de-gating

d) Minimal number of core boxes

e) Simple easy to understand design

2) A 3D model is drafted to reflect the above criteria Figure 13

3) A mold filling analysis is performed for gating verification Figure 12

a) Mold filling criteria are derived from gating calculations

i) 2500oF pour temperature

ii) 8 second fill time

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 iii) 28lb pour weight

Water Cooled Mold Creation

1) Incoming water flow rate is measured from the tap water faucet to be used Table 1

2) A pressurized 6 channel water distribution system is calculated, each channel shall rest below

a row of samples as they would be poured against the copper plate Table 3

3) A CAD model is drafted in Solidworks 3D CAD software representing all machined and

added features of the mold Figure 14

4) Copper plate, cast iron block, hose fittings, hardware, and liquid gasket are procured Table 2

5) 3D Cad drawing is imported into Mastercam CAM Software for tool path generation

6) The cast iron block is first mounted on the 2 Axis Milltronics Mill

7) Using hole center locations, counter bored bolt head holes are machined using the circular

pocket feature

8) Waste plate mounting holes and through block bolt holes are drilled using hole center

locations

9) Waste plate mounting holes are then tapped with a 5/16 x 18 bottoming tap

10) The cast iron block is mounted to a piece of waste plate and coordinated in the 4 axis

Milltronics mill

11) The CAM program is loaded into the 4 axis Milltronics mill and run

12) Once completed on the 4 axis machine. the cast iron block is then clamped on edge on the 2

axis Milltronics Mill to have channel inlet and outlet ports drilled

13) Inlet and outlet ports are then tapped and deburred Figure 15

14) Hose barb connectors wrapped in Teflon tape are threaded into the inlet and outlet channels

15) Next the copper plate is clamped to the bed of the 4 axis Milltronics mill and coordinated

16) The drilling program is loaded into the 4 axis Milltronics mill and run

17) Drilled holes are then tapped with a 3/8 x 16 bottoming tap

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18) Burrs are removed from all machined areas with a sharpening stone on the cast iron block

19) Raised areas of the copper plate are filed flat

20) The mating surfaces of the copper plate and cast iron block are cleaned with brake cleaner

21) Liquid gasket is applied around the water channels and bolt holes

22) Bolts containing both a washer and lock washer are threaded through the cast iron block and

into the copper plate and hand tightened.

23) The mold is allowed to cure for 24 hours Figure 16

24) Bolts are then torqued to 100 in/lb in a pattern in an alternating pattern from the outside to

the inside in quarter turn increments

25) The hoses are attached and the mold is then pressure tested to check for water-tightness

26) Water flow rate leaving the mold is measured and recorded Table 1

27) A cost analysis of the water cooled mold construction is then verified Table 2

Core Box Creation

1) Sample and gating designs are broken apart in Solidworks and drawn into uniform core

boxes that are large enough for easy stack mold creation later on.

2) The core box designs are then verified against each other for consistent feature placement

3) CAD files are then loaded into Mastercam for tool path generation Figure 17

4) Red Board strips are arranged and epoxied together to form 3 blocks with the minimum

dimensions 13.5in x 16in x 1.5in

5) The block is then fly-milled on the back surface using the 4 axis Milltronics Mill at a depth

that provides a flat final surface.

6) A bolt hole pattern is then drilled into the back surface using a 1.5inch incremental step

command on the 2 axis Milltronics Mill

7) The holes drilled into the back of the block are then tapped with a 5/16 x 18 bottoming tap

8) The block is then mounted to waste plate with 5/16 x 18 countersunk head bolts

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9) The first block and waste plate are then mounted on the 4 axis Milltronics Mill and

coordinated

10) The axis are zeroed using an edge finder

11) Tools are loaded securely into the tool holders and tools height offsets are set against the top

of the waste plate

12) The CNC program is loaded onto the mill controller and verified and ran Figure 18

13) Steps 5-12 of core box creation are repeated for the next two core boxes using their

respective CNC programs

Mold Cart Creation

1) A cart is designed to hold the water cooled mold on Solidworks Figure 19

a) The design is specified by comfortable pour height and sand core size

2) 1.5in x 3/16 square tubing is then cut to size and dry fit around the water cooled mold

3) The cart is then welded together using a Miller Shopmaster wire welder Figure 9

4) Holes are drilled into the steel tubing at the same locations of the waste plate mounting molts

previously drilled into the cast iron block.

5) The water cooled mold is then bolted to the steel plate which is then welded in place

6) Casters are then fastened to the bottom of the cart

Making Sand Cores

**Thoroughly clean the Palmer continuous mixer after each core box**

1) Check for sufficient quantities of resin, 15 minute catalyst and sand on the Palmer Mixer

Figure 5

2) Gather all necessary molding tools and extra molding boards and molding gloves

3) Inspect the surface of the core boxes for debris or damage

4) Apply parting powder to the interior surfaces of the core box being sure to tilt the core-box to

apply parting power to the vertical surfaces

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5) Mix sand into a pail for between 15 and 25 seconds depending on the core box

6) Dump the sand into core box

7) Begin molding a core starting at the outside edges

8) Press sand into the deep areas by applying pressure with fingertips

9) Mold around the perimeter of the core and then work inward

10) To compact the interior passages, mold in the same fashion as the perimeter working in

straight lines

11) Disperse any remaining sand over the top of the core box and compact with the palm of your

hand

12) Strike off the top surface immediately after molding is completed Figure 20

13) Tap the side of the core box lightly on all 4 sides to help remove the core from the core box

a) Be careful not to tap too hard or the core will fracture and later break

14) After 5 minuets check the sand strength by pressing lightly on the surface of the core

15) If the sand cured properly it should be strong enough to be removed with ease

a) Removing the core too soon will result in the core crumbling from the core box

b) Waiting unnecessarily long to remove the core will result in the core sticking in the core

box and needing to be broken out

16) Place a large molding board on top of the core box

17) Grasp the board and core box and flip them both over being careful not to drop the core box

18) Set the board and upside down core box on the Palmer vibrating molding table Figure 4

19) While holding the core box against the board, vibrate the core box for 15 seconds

20) Using light fingertip pressure, attempt to lift the core box off the core

a) It helps to squat down and look along the molding board surface to watch the core drop

b) Rock the core box forward and back and left to right slightly to help the core drop

c) If the core continues to stick, try to vibrate the core box again

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 d) If the core continues to stick try tapping the back of the core box

e) As a last measure to remove the core lift the molding board and core box up to a height of

2-3 inches and thrust them downward at the table

i) This method should be used as a last resort, it can easily break the core

f) Once the core is removed, transfer it to a smaller molding board and store in a safe, level

place

g) Repeat core making procedures for all remaining core boxes

i) The core containing the direct pour riser is currently loose molded in a steel frame as

it awaits larger core box creation

ii) Mold at least one more of each core to be safe if one should break

h) Molds can be dried in a microwave oven to aid removal of moisture Figure 21

i) It is best to let cores set-up for at least 24 hours on a well ventilated rack to permit

adequate binder strength

Assembling the Sand Mold

1) Gather all 4 premolded sand cores, level, and an air hose and nozzle

2) Position the mold cart in a convenient location and route hoses out of the way

3) Check the surface of the mold cart with a level, adjust if necessary

4) Using your fingers, rub all edges of the cores to remove any sand fins

5) No core glue is to be used between mold layers, instead the layers are to be rubbed together

to form a tight seal

6) Begin by rubbing the bottom side of the sample core against the copper plate, rub in a tight

circular motion

7) Next, with the sample core oriented on the copper plate, rub the bottom of the gate core

against the top surface of the sample core

8) Position the gate core correctly on the sample core

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9) Continue the same process, rubbing the runner core and pour cup core against the core that

will sit below it

10) Carefully disassemble the mold assembly and blow off the copper plate

11) Now reassemble the fitted cores back in position, blowing off each core before adding it to

the mold Figure 22

12) Add at least 200lbs of mold weights to the top of the mold

13) Cover the pouring basin to prevent debris from entering the mold

14) Green sand can be packed around the mold if desired Figure 23

a) Packing green sand around the mold will increase the mold change time, or only allow

one pour per heat

Pouring a Heat

1) A melt procedure has been posted in the UW-P foundry and the procedure found therein is

what will be used to melt Table 8

a) A melt pour and temperature log must be kept Table 5

i) The melt procedure may be different for each foundry and furnace charge material,

always follow the same melt rates to achieve a high level of consistency

ii) Data should be collected and logged to establish more accurate melt data and data

comparisons

b) Remember to pour a chill wedge and spectro button

i) Chill depth on the chill wedge should also be recorded

c) If pouring multiple heats in succession there is no need to preheat the furnace lining and

melting may begin immediately

Preliminary Analysis

1) A chill wedge should be sectioned and its chill depth recorded

2) Sample locations are then marked with a paint or permanent marker Figure 24

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Statistical Analysis and Chemistry Certification

1) Chemistry certification criteria are determined by each individual company requesting

samples

2) Certification should follow appropriate statistical sampling sizes

a) Reference ASTM publication E 1724-95 Standard Guide for Testing and Certification of

Metal, Ores, and Metal-Related Reference Materials

b) Once enough heats have been poured to assure process consistency, a reduced number of

samples may be tested if desired

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 Data

Table 1 Water Flow Rate Into and Out of the Water Cooled Mold, Measured by Weighing Water
Collected In a 5 Gallon Pail over a 10 Second period, Average Amounts Shown Below

Measured Flow Rate

Weight Time
(lbs) Gallons (sec) Gal/Min

Input Rate
17.1 2.06 10 12.36

Output Rate
15.78 1.90 10 11.41

Table 2 Cost Breakdown of Building the Water Cooled Mold

Water Cooled Mold Cost

Individual Unit Manufacturer/
Part Quantity Description
Cost Cost Distributor
Cold Rolled 110 Cu Plate 12 x Copper and
Copper Plate 1 565.09 565.09 12 (+,-.063) x 1 in (+,- .024) Brass Sales
12.25 x 12.25 x 2in Continuous
Cast Iron Plate 1 129.73 129.73 Cast Gray Iron Slab (Donated) Dura-Bar
Threaded Hose 1/2in NPT - 5/8 ID Hose Barb
Barb 2 2.63 5.26 ACE Hardware
Liquid Gasket 1 3.38 3.38 RTV Silicone Sealant, 650oF Permatex
Hose Clamps 3 0.59 1.77 1in Diameter ACE Hardware
Hose (per foot) 25 0.54 13.50 5/8in ID Radiator Hose ACE Hardware
Teflon tape (per 1/2in Wide Teflon Tape Roll,
roll) 1 2.59 2.59 25ft ACE Hardware
3/8in Dia x 2 3/4in x 16
Bolt 16 0.30 4.78 Threads/Inch, Grade 5 Fastenal
Lock Washer 16 0.03 0.45 3/8in Dia Fastenal
Washer 16 0.04 0.66 3/8in Dia Fastenal

Total Cost 727.2

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Table 3 Water Cooled Mold Coolant Channel Calculations Spreadsheet Screenshot

Table 4 Gating Calculations Spreadsheet Screenshot

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 Table 5 Melt Log for 4-26-07 Ductile Iron Melt

Melt Log 4-26-07

Actual Scheduled
Event
Time Time
Charge returns, Preheat lining
10:39 0:00 (Begin preheating treatment vessel ductile only)
11:40 1:00 Increase power to begin melting
12:00 1:20 Charge pig, all returns have been charged
Charge graphite, FeSi, FePhos, FeCr, Etc and begin
12:20 1:40 charging steel, all pig has been charged
12:45 2:00 All charge melted, increase bath temperature to 2800oF
Deslag melt, pour thermocouple cup to verify carbon and
12:55 2:15 silicon content, add graphite or FeSi as necessary
1:20 2:30 Prepare treatment vessel and treat iron (ductile only)
1:25 2:35 Pour chill sample mold, final thermocouple cup
1:30 2:40 Sand mold removed from copper plate

Temperature and Event Log

Time Temperature Event, mold pour times, chill wedge chill depth
12:45 2750
12:55 Prelim Thermocouple Cup C:3.7 Si: 2.3
1:05 2775
1:17 2835
1:20 2870 Tap Furnace into Treatment Vessel
Pour Chill Sample Mold, Spectro Button and Chill Wedge
1:25 2535 Depth .4in, No Final Thermocouple Cup Poured

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Table 6 Iron Heat Chemistry for the Second Sample Heat

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Table 7 Iron Heat Final Chemistry Continued From Table 6

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 Results

First Pour Results

Chill depth within the first pour appeared promising. Upon sectioning a sample a white iron

microstructure was observed unmagnified as fractures exposed a dendritic structure extending

half the height of the sample. After polishing and examination of the microstructure it was

determined the samples were unsuitable for use as standards due to the presence of graphite

nodules interlaced into the dendrite arms. Reason suspect for this occurrence has thus far been

poor melt practice, resulting in the late and unintentional inoculation of the bath just before and

during magnesium treatment. A second test heat has been scheduled and will attempt to

eliminate the presence of the nodules via strict melt practice. Thus far, no additives such as

Tellurium and Bismuth have been utilized to induce chill.

All samples have filled and have no shrinkage along the chill surface.

Samples were easily removed from the gating system, however they contained much burn-on and

cannot be run through a shot-blast machine for fear of removing the sample markings applied

with a paint marker.

Water condensation was observed on the copper plate from the sand cores after iron was poured

into the mold. This occurrence would hinder multiple pours in rapid succession because of the

safety hazards imposed. A longer cure time may be the remedy for this situation, or the use of a

long preheating cycle in a microwave oven to drive moisture from the mold.

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Second Pour Results

For the second heat, backing sand was not packed around the sand mold. A run out was then

experienced as a corner of the runner mold broke out as the runners filled with iron. Backing

sand was intentionally avoided to determine how the mold would react and determine the

viability for a run out between the mold layers. An in layer breakout was not expected and its

occurrence fostered questions about binder choice. A possible remedy for this situation would

be to use backing sand around every mold, or attempt a different sand binder with a lower

expansion characteristic.

The pour event and temperature log can be found in Table 5. The melt progressed without

incident and occurred at a faster pace than predicted.

Samples contained significant cold lapping and a sunken center section along the chill surface.

A slow pour time and a run out in runner bar core may be to cause for this.

Samples were easily removed from the gating system and present the same challenges in

marking and cleaning as experienced in the first heat.

Water condensation was again experienced upon the copper plate even after a 2 day core curing

period.

A chemistry calculation found in Table 6 was in error due to the absence of a silicon recovery

rate in the properties table; this mistake increased the silicon value by .5%, the chemistry

calculator appeared correct for the other elements.

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Polishing and examination of the microstructure shows a presence of type I to type V graphite

nodules among a white iron dendritic structure, however in fewer quantities than experienced in

the first heat. Further examination also shows the presence of micro cracks and shrinkages

throughout the sample and also localized around the in-gate. Further research should be

conducted on the affect of these cracks on sample integrity and on the presence of the graphite

nodules and the use of a chill inhibiter to prohibit the formation of graphite in ductile iron.

Discussion

Sample Design Considerations

The sample diameter was chosen based upon existing RM standard sizes, and increased slightly

to maximize use of the available surface area of copper plate while still allowing a minimum of

.25in sample spacing for sufficient sand core strength.

The sample height was chosen to be 3/4in based upon test heats which took place months before

the sample design. In those tests a maximum chill depth of .25in was observed against an

uncooled copper plate. Following that observation the original sample design having 1in height

was reduced to eliminate extra metal volume and consequently extra heat which would need to

be dissipated. A sample height less that 3/4in may produce a microstructure containing deeper or

even complete chill, however this has yet to be investigated and has thus far been deemed

unnecessary as the samples were designed to be hand ground and should keep a rather tall

appearance.

Improvements to the Current Setup

Quick Change Mold System

A mold securment system has been suggested a novel idea to allow for the pouring of sequential

molds. Molds may be assembled elsewhere and then quickly placed upon the copper plate as a

single unit. Ideas to secure cores together include through bolts or a key core molded around the

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entire assembly. After a short 5 minuet cool down on the copper, the assembled sand core

package could be slid out of the way and another assembled mold may be placed on the copper

plate. This method would increase the number of pours per heat, and could be used to produce

samples of intentionally varying magnesium content in ductile iron. Temperature of the water

flowing through the water cooled mold experienced a minimal increase; the mold could easily be

used for rapid pours without taxing the heat removal rate of the system.

Permanent Sample Markings

A permanent method for sample marking needs to be implemented. The current core boxes have

no surfaces available for engraving permanent sample markings because of the current parting

plane locations. A possible remedy for this may include the utilization of core-blowing instead

of hand packing. In such a process the existing gate and sample molds could be mated together

to form a single core, this would allow the samples core box to be engraved with the sample

location.

Sand Binder Choice

The sodium silicate binder system employed at the University of Wisconsin-Platteville has

serious limitations when used with high mold temperatures such as those experienced when

pouring iron. Molds are prone to cracking and the binder hardens significantly upon

experiencing high temperatures facilitating difficult mold removal. To alleviate this problem a

different binder system designed for high temperature use should be utilized.

Sample Core Box Material

The idea of eliminating the bottom sample core box and instead using a machined copper plate

has been suggested. This approach may provide the opportunity for increased chill depth if

needed. One foreseeable consequence to this approach is the sample contraction away from the

copper walls as it cools which could result in uneven chill depth.

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Conclusion

Production of spectrometer standard samples in small batches appears promising although

further research is required to refine aspects such as choice of binder systems and mold

construction techniques. The process shows potential at producing rapid succession pours for

fast production of samples.

References

Preparation of NBS White Cast Iron Spectrochemical Standards, U.S. Dept. of Commerce,
National Bureau of Standards, Misc. Publication 260-1, Issued June 19th, 1964.

Spectrometric Standards. Project 169, Metals Research and Development Foundation, Prepared
by Price Burgess, April 15th 1983

Tentative CRM Production Method, Iron Casting Research Institute Ad Hoc task group lead by
Pete Meyst, Oct. 15th 2002

Standard Practice for Testing Homogeneity of Materials for Development or Reference

Materials, American Society for Testing and Materials, E 826-85 (Reapproved 1996)

Standard Guide for Testing and Certification of Metal, Ore, and Metal-Related Reference
Materials, American Society for Testing and Materials, E 1724-95 (Reapproved 2001)

Standard Guide for Planning, Carrying Out and Reporting Traceable Chemical Analysis of
Metals, Ores and Related Materials, American Society for Testing and Materials, 2053-00

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Appendix A

Figure 10 3D Model of Sample Size and Figure 11 Sample Layout on the Copper
Specifications, Samples Include 5 Degrees Plate
of Draft

Figure 12 Solidcast Mold Filling Analysis Screenshots

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 Figure 16 Assembled Water Cooled Mold
Waiting for the Gasket Sealer to Cure

Figure 13 3D Model of the Gating System as

it would Rest on the Copper Plate

Figure 17 MasterCAM Toolpath

Visualization for the Samples Core box
Figure 14 3D Model of the Cast Iron Block
as it would Contain Coolant Passageways
and Bolt Holes

Figure 18 Machining of the Runner-Bar

Corebox

Figure 15 Machined Cast Iron Block

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Figure 19 3D Model of the Mold Cart

Figure 22 Assembled Sand Mold

Figure 20 Sand Core yet to be Removed

from the Core box

Figure 23 Assembled Sand Mold Ready to

Pour

Figure 21 Sand Cores Awaiting Mold

Assembly

Figure 24 First Set of Standards Cast on

4-12-07

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Table 8 Tentative UW-Platteville Iron Melt Procedure

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