Entegris SemiChem APM 2000 Guida utente

ADVANCED MATERIALS HANDLING |APPLICATION GUIDE

SemiChem APM 200 with HF and

H2O2in DSP+

Application guide

2Application Guide | Entegris, Inc.

SEMICHEM APM 200 WITH HF AND H202IN DSP+

TABLE OF CONTENTS

—

Introduction ........................................................................ 3

A.1 Precautions................................................................... 3

A.2 Reassembly................................................................... 3

A.2.1 Start-up Kit .............................................................. 3

A.2.2 Glass Burettes......................................................... 4

A.2.3 Reagents and Tubing............................................ 5

A.2.4 ORP and Fluoride Sensors .................................. 5

A.3 Preparing to Run......................................................... 6

A.3.1 Facilities .................................................................... 6

A.3.2 Flush Burettes......................................................... 6

A.3.3 Settings..................................................................... 6

A.3.4 Recipes and Adjustments.....................................7

A.3.4.1 Recipes..........................................................7

A.3.4.2 Adjustments................................................ 8

A.3.5 ORP Sensor Calibration ..................................... 12

A.3.6 Fluoride ISE Sensor Calibration ....................... 12

A.3.6.1 Auto Cal Adjustments ............................ 13

A.4 Running ........................................................................13

A.4.1 First Run.................................................................. 13

A.4.2 Process Calibration ............................................. 14

SEMICHEM APM 200 WITH HF AND H202IN DSP+

3Application Guide | Entegris, Inc.

INTRODUCTION

—

Our SemiChem APM 200 (advanced process monitor)

application guide provides step-by-step instructions

for properly conﬁguring the SemiChem APM 200 for

the DSP+ application for measuring low level HF and

hydrogen peroxide only. This guide is designed for

trained and qualiﬁed personnel. It is complimentary

to the SemiChem APM 200 Installation and Operating

Manual, not a replacement.

A.1 PRECAUTIONS

—

Be sure any personnel working on the SemiChem

APM 200 has read and understands the Installation

and Operating Manual. There are inherent hazards

to working with the SemiChem APM 200.

WARNING: Service of the SemiChem APM 200

may cause exposure to hazardous conditions

including chemical, electrical, and mechanical

dangers. Personnel should be properly trained

in all areas before attempting to service or

troubleshoot the analyzer.

WARNING: Electrical Precaution: High

voltage electronics (⁄ VAC) are located

throughout the electronics module. Printed

circuit boards are powered with 24 VDC. All

service should be performed by a qualiﬁed

electrician/electrical technician.

WARNING: Chemical Precaution: Corrosive

or poisonous liquids. Some reagents may

be corrosive to the eyes, skin, and respiratory

tract and may be hazardous if ingested. Wear

chemical resistant gloves, face shield, and

apron when changing the burette O-ring. See

MSDS for further health hazard information.

To minimize chemical exposure, purge the

burette with air by removing the reagent intake

line from the reagent bottle, then ﬂush the

appropriate burette. This will remove most

of the reagent from the burette assembly.

If replacing the burette glass, consult with

on-site environmental personnel for proper

disposal of remaining reagents. If replacing

a burette O-ring, keep the burette glass

assembly within the enclosure for proper

exhaust of fumes.

It is the user's responsibility to fully understand the

use, application, and hazards associated with the

SemiChem APM 200. Refer to the SemiChem APM 200

Installation and Operating Manual for more information.

A.2 REASSEMBLY

—

A.2.1 START-UP KIT

To complete the start-up of the SemiChem APM 200,

you will need:

1. 1 ea. ⁄” ball driver (003642).

2. 4 ea. tube weights and barbs (001824 and 003529).

3. Silicone paste kit (002691).

Start-up kit items.

SEMICHEM APM 200 WITH HF AND H202IN DSP+

Application Guide | Entegris, Inc.

In addition, you will need:

1. Glass burettes (000503) – the number of glass

burette assemblies will vary depending on

the application.

2. 8 – 32 × ⁄” SHCS (000762-050).

3. The sensor, Electrode, ORP Combination (001836) and

the sensor Electrode, F-, ISE Half Cell (001770).

A.2.2 GLASS BURETTES

Burette installation:

1. Using the silicone paste kit, apply a small amount

of silicone to each burette piston’s O-ring.

NOTE: Silicone paste is not needed on jacketed O-rings.

2. Install the glass burette into the piston and

guideposts using a slight twist motion.

3. Secure the burette glass assembly with the

8 – 32 × ⁄” SHCS and ⁄” ball driver.

4. Repeat for burettes 2 and 3.

Installed burettes.

SEMICHEM APM 200 WITH HF AND H202IN DSP+

5Application Guide | Entegris, Inc.

A.2.3 REAGENTS AND TUBING

Reagents installation:

1. Within the reagent storage, locate and uncoil the

reagent tubing.

NOTE: Each reagent tube is labeled with its

corresponding burette.

2. Insert the barb into the tube weight.

3. Remove the reagent cap from the reagent bottles

and slide the reagent 1 tube through the cap.

4. Install the barb/tube weight combination onto the

end of the reagent tube.

5. Repeat for reagents 2 and 3.

Installed tube weight.

6. Fill each reagent bottle with the reagents:

– Reagent bottle 1: 500 ppm ﬂuoride

standard

– Reagent bottle 2: TISAB buer

– Reagent bottle 3: 0.25 N ceric sulfate in

1.0 N sulfuric acid

7. Carefully insert the tube weight/tube/cap

combination into corresponding reagent bottle.

Be sure the tube weight falls to the bottom and

sits ﬂat. Secure the cap. Place reagent bottles

into the corresponding slots within the reagent

storage area.

NOTE: To follow the recipe parameters it is important that

the reagents are correctly assigned to the proper burettes.

A.2.4 ORP AND FLUORIDE SENSORS

1. Remove any caps and covers on the ORP sensor.

NOTE: There may be residual white crystals. These

crystals are saturated potassium chloride solution.

They are normal and can simply be wiped away.

2. Remove all caps and covers on the ﬂuoride ion

selective electrode (ISE).

3. Remove the electrode retaining nut(s) from the

measuring cell. Remove the 3 mm × 11 mm O-ring

from the electrode port. You can choose to use any

of the open ports.

4. Slide the electrode into the retaining nut. Be

careful, the electrode is glass and can break.

Slide the O-ring onto the electrode shaft.

5. Insert the electrode/retaining nut/O-ring

combination into the measuring cell.

Repeat for the ﬂuoride ISE.

6. Locate the electrode cable labeled “Input 1”.

Connect the ORP electrode and the electrode

cable. Locate the electrode cable labeled “Input 2”.

Connect the ﬂuoride ISE and the electrode cable.

NOTE: To follow the recipe parameters it is important

that the electrodes are connected to the proper inputs.

Fluoride ion selective electrode with protective cap.

ORP electrode with protective cap.

SEMICHEM APM 200 WITH HF AND H202IN DSP+

Application Guide | Entegris, Inc.

A.3 PREPARING TO RUN

—

A.3.1 FACILITIES

At this point, the SemiChem APM 200 should be

fully installed and reassembled. All utilities can now

be energized.

1. Close all doors and be sure the exhaust is

connected and active.

2. Power up the SemiChem APM 200. The SemiChem

APM 200 information system will turn on. The MAIN

screen will be available shortly.

NOTE: If the system has been provided with safety

interlocks, the screen will have a RED background

indicating the safety interlocks require a reset. Press the

"GREEN" button below the EPO button to initiate the

safety circuits. Once pressed, and all safety interlocks

have been satisﬁed, the system is now ready.

3. Turn on CDA, water, and sample. Visually verify

there are no leaks.

4. From the MAIN screen, press "Service," then

press "Recipes."

5. From the service screen, select the recipe "Flush Cell."

Press "Run Now."

6. Verify water sprays into the cell from the top. It will

spray into the cell with the drain open for about 20

seconds, the drain closes and the water level will

reach the level sensor and stop the spray.

Service > Recipes.

Entegris / Service / Recipes

Recipe Menu:

Edit

New

Delete

Set As Main

Run Now

Done

Recipe Name

HF and Total Acid Sample 1 and 2

HF and Total Acid Sample 1

HF and Total Acid Sample 2

Flush Cell A

Empty Cell A

Flush Burette 1

Flush Burette 2

Flush Burette 3

Flush Burette 4

Flush All Burettes

Homemotors

Import

HF and H2O2 Sample 1 and 2

HF and H2O2 Sample 1

HF and H2O2 Sample 2

H2O2 in CMP Slurry Sample 1

H2O2 in CMP Slurry Sample 2

A.3.2 FLUSH BURETTES

Flushing the burettes with the appropriate reagents:

1. From Recipes, choose "Reﬁll_Burette_1." Press

"Run Now." The burette will proceed to cycle

up and down three times. During which, it will

displace the air in the burette with the reagent.

Once complete, the reagent tubing and glass

burette will be completely ﬁlled with reagent.

Repeat for burettes 2 and 3.

2. Carefully inspect the burette glass and all tubing to

verify that all the air and bubbles have been purged

from the burette system. If not, repeat the above

step. For proper performance, the burette system

must be completely free from air bubbles.

3. Select "Flush_cell." Press "Run Now."

A.3.3 SETTINGS

The SemiChem APM 200's operation and behavior

within a process environment can be conﬁgured

to suit speciﬁc user needs. The settings allow the

SemiChem APM 200 to ﬁt into the user’s process

control systems. There are eight setting screens.

Use the following to program the settings. Refer to

the “Software Flow Chart” in the SemiChem APM

200 Installation and Operating Manual for more

information on each setting.

1. From the MAIN screen, press "Service," then

press "Settings."

Service/Settings.

Entegris / Service / Settings

OK Cancel

Back Next

Labels

Analog Outputs

Channel 1-4 Configuration

Channel 5-8 Configuration

Calibration Data / Trigger / Calculation Factors

pH Buffer Concentrations

Remote Input Triggers

Analysis Timing

Channel 2 Label

Channel 3 Label

Channel 4 Label

Channel 5 Label

Channel 6 Label

System Date / Time

SEMICHEM APM 200 WITH HF AND H202IN DSP+

7Application Guide | Entegris, Inc.

Labels: The “Labels“ menu is used for labeling the

SemiChem APM 200. As an example:

– Burette 1 Label: Fluoride Standard

– Burette 2 Label: TISAB

– Burette 3 Label: 0.25 N Ceric Sulfate

– Sample 1 Label: Tank 1 DSP+

– Sample 2 Label: Tank 2 DSP+

– Output 1 Label: HF Tank 1

– Output 2 Label: Hydrogen Peroxide Tank 1

– Output 3 Label: HF Tank 2 (if used with the

dual sample system option)

– Output 4 Label: Hydrogen Peroxide Tank 2

(if used with the dual sample

system option)

Analog Outputs: Sets the range for each output.

NOTE: The SemiChem APM 200 utilizes 4 – 20 mA analog

signals. 4 mA will be 0, 20 mA will correspond

to the high range.

Relays: Sets the behavior and threshold for each alarm.

Calibration Data/Trigger/Calculation Factors:

1. Trigger: If set to local, the SemiChem APM 200 will

run independent and will run whichever recipe

is set as default based on the internal analysis

frequency. If set to remote, the SemiChem APM

200 will run with PLC handshaking. In addition,

the user can select which recipe to run when using

the recipe select feature. If set to computer, the

SemiChem APM 200 will respond to commands

from the RS232. Refer to the SemiChem APM 200

Installation and Operating Manual, section 4.2.

2. Calculation Factors: These are set as part of the

process calibration.

pH Buer Concentration: When using an ORP

electrode, these are not used.

Remote Trigger Inputs: Each remote trigger input

can be tied to a recipe. Therefore, when either a

PLC (remote mode) or a PC (computer) send the

input (as per the SemiChem APM 200 Installation

and Operating Manual, section 4.2) the SemiChem

APM 200 will run the recipe tied to the input. For

example, Remote Recipe 0 may be the "HF and

Hydrogen Peroxide in Sample 1" recipe, and Remote

Recipe 1 may be the "HF and Hydrogen Peroxide in

Sample 2" recipe, and Remote Recipe 1 may be the

"HF and Hydrogen Peroxide in Sample 2" recipe.

In this case, the user can select which analysis

to perform depending on the control needs of

the process.

Analysis Timing: Sets the analysis frequency and sensor

equilibration time.

NOTE: The SAMPLE TRANSFER VOLUME must be set to

whatever the cell volume is in milliliters. This is typically

set to 200.

System Date and Time: Sets the date and time.

A.3.4 RECIPES AND ADJUSTMENTS

A.3.4.1 Recipes

The SemiChem APM 200 is provided with a variety of

recipes as a set of application defaults. These recipes

should be considered “starting points” and will most

likely need to be adjusted to meet individual needs.

The recipes available for the DSP+ process for HF and

H2O2are:

HF and Hydrogen Peroxide Sample 1: This recipe will

measure both HF and Hydrogen Peroxide in series on

sample 1 only.

HF and Hydrogen Peroxide Sample 2: This recipe will

measure both HF and Hydrogen Peroxide in series on

sample 2 only.

HF and Hydrogen Peroxide Sample 1 and 2: This recipe

will measure both HF and Hydrogen Peroxide in series

on sample 1 and sample 2.

AutoCal channel 2: This recipe sets the calibration

parameters to calibrate the ﬂuoride ISE on input 2.

HF self test: This recipe allows the user to conﬁrm

the operation of the ﬂuoride ISE by creating an

internal sample.

SEMICHEM APM 200 WITH HF AND H202IN DSP+

Application Guide | Entegris, Inc.

A.3.4.2 Adjustments

Once the desired recipe is selected, there are a number of parameters that can be adjusted to optimize the perfor-

mance of the SemiChem APM 200. As an example, the recipe shown below is for HF and H2O2for Sample 1.

# Recipe: APM 200 HF and H2O2Sample 1

# Process: HF at 300 ppm, SHydrogen Peroxide at 4%

# Loop Size: 1 mL

# Burette Assignments: 1.500 ppm Fluoride Standard 2. TISAB Buer 3. 0.25 N Ceric Sulfate in Strong Acid

# Sensor Inputs: 1. ORP 2. F ISE

# Output Assignments: 1. HF in ppm 2. Hydrogen Peroxide in %

function main

# HF Analysis

call HOMEMOTORS motor1=yes motor 2=yes motor3=yes motor4=no

call CONDITION number=2 volume=0.25 valve=EV02

These recipes can be edited and adjusted. Additionally,

recipes can be imported via the USB.

Text notations of the recipe assumptions are within

each of the recipes. These assumptions are based on

the SemiChem APM 200 conﬁguration, the sample

loop volume, the burette assignments, the electrode

input assignments, the reagent concentrations, and

the process concentration range. Generally, it is

assumed that:

1. Sample loop is 1.0 mL. This is the factory default.

2. Burettes and electrode are assigned as per A.2.3

and A.2.4 (page 5).

3. Fluoride standard is 500 ppm and Ceric Sulfate

is 0.25 N.

4. The expected HF concentration is 300 ppm, and

the Hydrogen Peroxide expected concentration

is 4%. If the expected concentrations vary the

system conﬁguration and reagent concentration

may need to be adjusted. Please contact Entegris.

for more information.

SEMICHEM APM 200 WITH HF AND H202IN DSP+

9Application Guide | Entegris, Inc.

call CONDITION number=3 volume=0.25 valve=EV03

call BURETTE number=1 action=setvol volume=0.00 valve=EV01

call BURETTE number=2 action=setvol volume=0.00 valve=EV02

call BURETTE number=3 action=setvol volume=0.00 valve=EV03

call EMPTY_APM200_CELLA time=15

call FLUSH_APM200_CELLA time=25

call EMPTY_APM200_CELLA time=15

call SAMPLE time=8 valve=AV01

call TRANSFER_APM200_CELLA time=6000

call CONTROLIO io=MIXERA value=1 time=0

call TITRATE cell=1 number=3 channel_id=2_sensor_ch=1 endpoint=850 window=1.00 end=10.5 sensor=pH

algorithm=seek_set direction=up_1 min_inc=.03 max_inc=.4 goal=4.1 formula=normal units=mL oset=0.00 equib=3

call CONTROLIO io=MIXERA value=0 time=0

call CONDITION number=2 volume=4 valve=EV02

call CONTROLIO io=MIXERA value=1 time=10

call ISE cell=1 number=1 channel_id=1 sensor_ch=2 ph_sensor_ch=1 addn_mode=default meas_mode=ﬁxed

meas_time=30 cell_volume=200 std_conc=500 units=ppm def_conc=.75 factor=9 sensor=mV cal=no cal_ch=1

call EMPTY_APM200_CELLA time=15

call FLUSH_APM200_CELLA time=25

call EMPTY_APM200_CELLA time=10

call CONTROLIO io=MIXERA value=0 time=0

call FLUSH_APM200_CELLA time=10

call HOMEMOTORS motor1=yes motor2=yes motor3=yes motor4=no

end

SEMICHEM APM 200 WITH HF AND H202IN DSP+

Application Guide | Entegris, Inc.

HOMEMOTORS: This brings the burettes motors to

their uppermost position.

CONDITION number=1 volume=0.25 valve=EV01:

Injects 0.25 mL of burette 1 using electric valve 1. This

essentially prepares the burette for use and clears the

reagent dispensing tip of any bubbles.

BURETTE number=1 action=setvol volume=0.00

valve=EV01: Resets the system’s tracking of the

volume of reagent injected.

EMPTY_APM200_CELLA time=15: Opens the drain

valve for 15 seconds. The time can be adjusted

to ensure that the drain fully empties prior to the

next step.

FLUSH_APM200_CELLA time=25: Spray rinses the cell

for 25 seconds. This time can be adjusted to ensure

the cell is completely rinsed prior to the next step.

SAMPLE time=8 AV01: This command prepares the

6-port valve to take a sample. Additionally, it opens

valve AV01, the sample 1 inlet valve, and diverts sample

to the 6-port valve for eight seconds. This time can be

adjusted to accommodate varying sample inlet ﬂow

rates. Note, the sample time only has to be long

enough for a fresh sample to go from the 3-way

recirculating AV01 to the 6-port valve.

TRANSFER_APM200_CELLA time = 6000: Prepares

the 6-port valve to deliver sample to the measuring

cell. Opens AV03 to transfer the contents of the

sample loop to the measuring cell. AV03 will remain

open until either the cell level sensor trip or the time

is reached. If the level sensor is not tripped within the

deﬁned time (6000 seconds), the system will respond

with an error code: 64.

CONTROLIO = MIXERA value = 1 time = 10: Turns

the mixer motor on. This is not adjustable.

TITRATE (for the H2O2measurement):

– cell = 1: Cell 1 in single cell system, cell 1 or 2 in

dual cell system.

– number = 3: Deﬁnes which burette is used to

perform the titration.

– channel_id = 2: Deﬁnes which displayed and

analog output is used for this measurement.

– sensor_ch = 1: Deﬁnes the ORP electrode is

connected to sensor input 1.

– endpoint = 850: Deﬁnes the titration endpoint

value. Can be optimized for the chemistry’s

endpoint.

– window = 100: Deﬁnes the tolerance in which

the SemiChem APM 200 will seek for the actual

endpoint. In this case, the SemiChem APM 200

will search from 750 to 950 for the endpoint.

– end = 1050: Deﬁnes when the titration

is terminated.

– sensor = mV: Deﬁnes the displayed sensor

graph scale.

– algorithm = seek/set: Deﬁnes how the SemiChem

APM 200 determines the endpoint. Seek allows the

SemiChem APM 200 to determine the endpoint

within the window. Setpoint assigns the endpoint

at a ﬁxed value. Seek/set allows the SemiChem

APM 200 to ﬁrst search for the endpoint within

the window. If unable, then it will revert to the

setpoint value.

– direction = up_1: Deﬁnes the direction of the

titration. It also deﬁnes the method of reagent

injection. Up value conﬁgures the reagent

injection volumes based on the slope of the

sensor response curve using the min. and max.

increments. Up-1 value conﬁgures the reagent

injection volumes based on a goal volume of

where the endpoint is expected.

– min_inc = 0.03 and max_inc = 0.4: Sets the range

of reagent volume injections. Min. increment is

usually 0.03. Max. increment is usually 10% of

the expected goal volume.

– goal = 4.1: When using the up-1 (or down-1)

titration direction, the SemiChem APM 200

will optimize reagent volume injections based

on the expected endpoint volume. As the total

reagent volume injections get closer to the goal

volume, the system will inject smaller and smaller

increments as it slowly approaches the endpoint.

Thus, giving the SemiChem APM 200 more data

points in the critical portion of the sensor response

curve to determine the most precise endpoint.

This value can be adjusted to match the expected

endpoint value. This feature is only suitable for

applications in which the process is fairly stable.

Indice

Manuali Apparecchiature di prova popolari di altre marche

SMART

SMART KANAAD SBT XTREME 3G Series Manuale utente

Agilent Technologies

Agilent Technologies BERT Serial Manuale utente

Agilent Technologies

Agilent Technologies N3280A Manuale utente

Vernier

Vernier Go Direct Voltage Manuale utente

Lifeloc

Lifeloc R.A.D.A.R. Manuale utente

Fluke

Fluke T5-600 Istruzioni per l'uso e l'installazione

Mercury

Mercury TSL01 Manuale utente

MAHA

MAHA MBT Series Manuale utente

Fuji Electric

Fuji Electric P-61 Manuale utente

ETC

ETC SealerAtor Manuale utente

Skyfine

Skyfine ETHYWAY V2 Manuale utente

Appion

Appion G5 Twin Manuale utente

PCB Piezotronics

PCB Piezotronics 8159-0112A Manuale utente

BW Technologies

BW Technologies MicroDock II Manuale utente

Sun Nuclear

Sun Nuclear 1027 Manuale utente

Biomark

Biomark HPR LITE READER Manuale utente

Hioki

Hioki 3169-20 Manuale utente

Ashcroft

Ashcroft ATE-100 Manuale utente

entegris SemiChem APM 2000 Guida utente

Manuali Apparecchiature di prova popolari di altre marche