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pH and ICP Techniques PowerPoint PPT Presentation


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pH and ICP Techniques. Clemson. Scoop 2 checks One blank Double scoop 6 samples Tag set with lab number, check, and blank positions. pH quality control checks. Two QC check samples Two samples at beginning, middle, and end of set Cross Check electrodes #1 and #2 . 1. 2. 3.

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pH and ICP Techniques

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pH and ICP Techniques

Clemson


  • Scoop 2 checks

  • One blank

  • Double scoop 6 samples

  • Tag set with lab number, check, and blank positions

pH quality control checks


  • Two QC check samples

  • Two samples at beginning, middle, and end of set

  • Cross Check electrodes #1 and #2

1

2

3

Quality control row


ck

  • Check both QC check values at beginning and within set

  • Check all double scooped samples at beginning, middle, and end of set

  • Buffer run - checks

  • Buffer run - blank (1:1, water:buffer)

End of run verification


  • Friday

    • clean out electrode filling solution

    • fill with water

  • Ultrasonic cleaner

  • Store in buffer pH 7 for the weekend

Maintenance


  • Monday

    • Take water out of electrode

    • Refill with KCl filling solution

  • Verify flow of KCl through filter

  • Refresh buffer solutions

  • Electrode (from Fisher)

    • Accumet rugged bulb pH combination electrode

    • 13-620-183A

Maintenance – cont.


  • Check B data since April 1, 2010

  • 115 continuous reads over a 2.5 month period

  • Rinse pH < 4.5 and > 7.0

  • NAPT value 5.15

  • Lab average 5.15

  • stdev 0.036

pH Check values


  • Two checks within the set

  • One blank

ICP quality control checks


  • Probe – Leeman Labs

    • Phone: 603-886-8400

    • Part number 902-00017

  • Check all tubing for cleanliness and kinks

  • Change pump winding tube when needed

  • Adjust pump winding clamp - look for smooth flow as sample travels though tube

Sample entry


  • Aspirate yttrium stock solution

  • Look for the tip of the red bullet

  • Adjust nebulizer gas flow rate

ARCOS

TJA

Nebulizer gas flow


  • Keep clean

    • Take apart to rinse out nebulizer and spray chamber parts

  • TJA – use cleaning wire

  • ARCOS

    • SeaSpray Nebulizer

    • Twister Spray Chamber

    • Cross Flow

ARCOS

ARCOS

TJA

Nebulizer and spray chamber


  • ARCOS – clean as needed – salt buildup

  • TJA – clean ~once a year

TJA

ARCOS

Torch


  • Transient scan – run standard

  • Check to see when the peak intensities stabilize

  • Clemson – 35 second total flush

    • 25 seconds at 60 rpm

    • 10 seconds at 30 rpm

25 seconds

P

K

Time (seconds) using pump speed of 60 rpm

Setting the flush timeARCOS - Crossflow


18 seconds

25 seconds

Crossflow spray chamber

Twister spray chamber

Transient scan on ARCOS


Options for changing flush time

  • Spray chamber

  • Tubing length

  • Pump speed

  • Sample loop

P – 100 ppm

Ca – 100 ppm

K – 100 ppm

Na – 50 ppm

45 seconds

25 seconds

Time in seconds using pump speed of 60 rpm

Transient scan going to rinseARCOS - Crossflow


  • Run time scan

  • Check time for stability

  • Clemson soil method

    • pump speed 200 rpm

    • flush time 30 seconds

Ca - 40 seconds

Pump speed 175 rpm

Setting the flush time - TJA


  • Look at several recommended lines

  • Clemson - Ca line – 317.933 for soil

Ca – 396.847Saturated signal

Ca – 315.887

Line selection – ARCOS


  • Set peak position

  • Select clean area for background subtraction

  • Look for uncontaminated blank

Peak position

Cu – 324.754

Blank correction

blank

Method development - ARCOS


  • Run profile when needed

  • On the AROCS - check intensity of P158.599 line

  • If significant UV intensity drop – clean window and/or lens to optics

  • Check new standard against old

  • Read reference sample at start, mid point, and end of run

  • Verify 2 check samples and blank within set

Instrument profile and data verification


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